Understanding the chemical and mineralogical composition of commercial henna and jagua tattoos and dyes-a multi-analytical approach.

Temporary tattoos and dyes constitute a great analytical challenge in relation to the regulatory control of their ingredients. Most of these commercial products are not labeled according to their content and their chemical nature is highly diverse. Therefore, it is necessary to analyze these complex samples to evaluate the potential presence of metallic impurities, to ensure the safety of cosmetic products contributing to health protection. This study proposes a multi-analytical methodology, which includes handheld X-ray fluorescence (h-XRF) and X-ray diffraction (XRD), complemented by variable pressure scanning electron microscopy coupled with energy-dispersive X-ray spectrometry (VP-SEM-EDS) to fully characterize 34 commercial samples of jagua and henna tattoos and dyes. The approach allowed the identification of the main constituents providing complementary compositional data and differences between sample types were established. In addition, information on the degree of natural pigments homogeneity was also obtained. The results' discussion considering the current European cosmetics regulation may be useful to support the drafting of safety requirements and specific regulation.

Evaluation and application of a new scintillator-based heat-resistant back-scattered electron detector during heat treatment in the scanning electron microscope.

A new high-temperature detector dedicated to the collection of backscattered electrons is used in combination with heating stages up to 1050°C, in high-vacuum and low-vacuum modes in order to evaluate its possibilities through signal-to-noise ration measurements and different applications. Four examples of material transformations occurring at high temperature are herein reported: grain growth during annealing of a rolled platinum foil, recrystallisation of a multiphased alloy, oxidation of a Ni-based alloy and complex phase transformations occurring during the annealing of an Al-Si coated boron steel. The detector could be potentially adapted to any type of SEM and it offers good opportunities to perform high-temperature experiments in various atmospheres.

Age related changes seen in human cornea in formalin fixed sections and on biomicroscopy in living subjects: A comparison.

The purpose of our experimental research was to assess the effects of aging on the main corneal structures in healthy corneas. Small, human cornea samples were collected from 20 Caucasian subjects during surgery for traumatic lesions to the eye. Ten subjects were adults (mean age 28 years) and 10 were elderly (mean age 76 years). Morphological analysis was carried out using light microscopy and electron microscopy. Another 40 patients (20 young: mean age < 30 years; 20 elderly: mean age > 70 years) were studied in vivo by confocal microscopy. The resulting images were analyzed qualitatively, quantitatively, and statistically. The basic light microscope revealed a decrease in endothelial cell density with age accompanied by an increase in endothelial cell size. Transmission electron microscopy revealed a corneal thinning and a decrease in the number of corneal stromal cells. A marked decrease in stromal nerve fibers was observed in the older subjects compared to the younger ones. Variable pressure scanning electron microscopy (VP-SEM) was used to make surface morphological observations and to determine the chemical composition of in vivo hydrated human corneas. Our results showed the effects of aging on normal corneal morphology highlighting the structural diversity of the corneal layers and revealing an age-related reduction in nerve fibers, thus explaining the decreased corneal sensitivity that may be observed in the elderly. Clin. Anat. 33:245-256, 2020. © 2019 Wiley Periodicals, Inc.

Novel microscopy-based approaches to study the film formation mechanism and associated mechanical response in polymer lattices.

In this paper, we present the results from novel microscopy-based approaches aimed at providing further insight into the mechanism of film formation and associated mechanical response in polymer lattices. Firstly, a 'simple' methodology, combining the use of variable pressure scanning electron microscopy and a recently introduced enhanced coolstage (-50 to +50°C), was successfully developed and not only used to study dynamic processes, e.g. different stages of latex film formation, but also for high-resolution imaging of 'freeze-dried' structures. By using the enhanced freeze-drying capability of the system, it was also possible to preserve the structure and features of the studied system with minimum shrinkage and distortion and in the case of polymer lattices at a desired stage of film formation. Moreover, specimens can then be readily imaged, without the need of conductive coatings and at much lower chamber gas pressures, thus minimizing the beam skirting effects and allowing higher resolutions to be achieved. The second and final part of our study consider the mechanical response of the studied latex dried under different conditions, with the particular emphasis on the effects of drying rate [% relative humidity (RH)]. Atomic force microscopy force distance curve measurements revealed that while the %RH did not have an effect on the structures formed, it did have an effect on the adhesive properties of the studied system. It is strongly believed that the methodologies developed and used here can be applied to other material systems, including biologicals and pharmaceuticals.

A Micro-Analytical Study of the Scarabs of the Necropolis of Vinha das Caliças (Portugal).

Five scarabs and one scaraboid found in Vinha das Caliças 4 (Beja, Portugal) were analyzed using a micro-analytical methodology in order to determine their mineralogical and chemical composition. Microstructural characterization and chemical analysis revealed that all were composed of a white body of crushed feldspathic sand covered by a lead-rich, alkaline-depleted silicate blue-green glaze showing evident signs of glass deterioration. Variable pressure scanning electron microscopy with X-ray energy dispersive spectrometry, handheld X-ray fluorescence spectroscopy, and micro X-ray diffraction results show that blue-green color of the glaze was produced by using copper ions (Cu2+) in conjunction with the lead antimonate bindheimite, a yellow-colored opacifier. The introduction of small amounts of tin in the structure of bindheimite enabled the production of a ternary Pb-Sb-Sn oxide. Tin, which was most likely added with the copper source (bronze scrapings), is known to facilitate the crystallization of bindheimite. The results are consistent with the five scarabs and one scaraboid being manufactured in Egypt. This study, the first archeometric study of scarabs found in the Iberian peninsula, has greatly contributed to the understanding of the influence of the Eastern and Central Mediterranean world in the Southwestern Iberia during the first millennium B.C.

Unveiling the Ambrotype: Characterization of Two 19th Century Photographs.

This work used a multi-analytical approach to characterize two 19th century ambrotypes and was motivated by the lack of insight on these historical objects. Photographic imaging and optical microscopy (OM) were used to identify abrasions, cracks related to reticulation, tarnishing, and other aspects associated to production and degradation processes. With variable pressure scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (EDS) these processes were seen with great detail and further characterized. Elemental point analysis and elemental mapping showed that the photosensitive material used was silver iodide. Degradation compounds were found as silver and chlorine-containing compounds. In one of the items, the tarnishing area also contained redeposited silver in a ring-shape surrounding a nucleus rich in silver, copper, and sulfur, in addition to copper-based salts. EDS analyses also identified that the supports were common soda-lime-silica glasses, refined with arsenic; and showed that a pigment rich in iron was used in both items to hand color the cheeks, extended with aluminum silicates alone or mixed with barium sulfate. The µ-Raman study pointed out that a synthetic Mars pigment was employed. µ-Fourier-transform infrared spectroscopy analyses identified collodion as the binder. Shellac was used as a protective varnish in one of the items and a gum was possibly employed on the other. Bitumen was used for the background in one ambrotype.

Environmental gas impact on the emission volume of X-rays near the interface in the variable pressure scanning electron microscopy.

In this paper, our previously developed model to account for the secondary X-ray fluorescence and absorption effects near the interface of two adjacent materials in a high-vacuum scanning electron microscope (Zoukel & Khouchaf, 2014) is adapted and extended to experimental conditions of low-vacuum mode (in the presence of a gaseous environment in the SEM analysis chamber). The position shifting effect of the two Gaussian peaks issued from the first derivative equation that can fit the experimental low-vacuum EDS profiles is investigated. The impact of the medium gas on the emission volume of secondary X-rays near the interface is qualitatively discussed. Water vapour and helium are successively used as gas environment, in order to link the resolution of microanalysis profiles with the effects of the X-ray fluorescence and absorption phenomenon. A close agreement between Monte Carlo simulation and experimental results is found.

Analysis of the Chemical Composition, Morphological Characterization, and Porosimetry of Allograft and Comparison with Xenograft for Dental Applications / Análisis de la Composición Química, Caracterización Morfológica y Porosimetría de Aloinjerto y Comparación con Xenoinjerto para Aplicaciones Odontológicas

SUMMARY: Tissue engineering aims to fabricate a scaffold that exhibits a suitable surface topography for a desired cellular response. Therefore, a study analyzing the characteristics of bone grafts is important for future research directions. This work aims to analyze the physical-chemical characteristics of commercially available bone grafts of human and bovine origin for dental use, using morphological analysis of the surface and chemical composition by variable pressure scanning electron microscope (VP-SEM) and energy-dispersive x-ray (EDX) spectrometry. In addition, pore diameter and surface area were analyzed by degassing method using a porosimeter, and particle size by laser diffraction. The analyzed allograft and xenograft particles differ in morphological characteristics and chemical composition. The allograft particles present a cuboidal and prismatic geometric morphology with angled edges and the absence of macropores. On the contrary, the xenograft particles present an irregular morphology with macropores in their structure. There is a statistically significant difference in C, P, and Ca between the xenograft and allografts (p < 0,05). The analyzed composition of allografts showed mainly the presence of C and O. In contrast, the composition of the xenograft was mainly Ca. These differences could influence the osteogenic properties of allografts and xenografts. This analysis provides basic information to understand the physicochemical properties of allografts and xenografts that facilitate cell-graft interaction.

La ingeniería de tejidos tiene como objetivo fabricar un andamio que muestre una topografía de superficie adecuada para una respuesta celular deseada. Por tanto, un estudio que analice las características de los injertos óseos es importante para futuros enfoques de investigación. Este trabajo tiene como objetivo analizar las características físico-químicas de injertos óseos de origen humano y bovino disponibles comercialmente para uso odontológico, mediante análisis morfológico de la superficie y composición química mediante microscopio electrónico de barrido de presión variable (VP-SEM) y x-dispersivo de energía. espectrometría de rayos (EDX). Además, el diámetro de los poros y el área superficial se analizaron mediante el método de desgasificación utilizando un porosímetro y el tamaño de las partículas mediante difracción láser. Las partículas de aloinjerto y xenoinjerto analizadas difieren en características morfológicas y composición química. Las partículas del aloinjerto presentan una morfología geométrica cúbica y prismática con bordes angulados y ausencia de macroporos. Por el contrario, las partículas de xenoinjerto presentan una morfología irregular con macroporos en su estructura. Existe una diferencia estadísticamente significativa en C, P y Ca entre el xenoinjerto y los aloinjertos (p < 0,05). La composición analizada de los aloinjertos mostró principalmente la presencia de C y O. Por el contrario, la composición del xenoinjerto fue principalmente Ca. Estas diferencias podrían influir en las propiedades osteogénicas de los aloinjertos y xenoinjertos. Este análisis proporciona información básica para comprender las propiedades fisicoquímicas de aloinjertos y xenoinjertos que facilitan la interacción célula-injerto.

Gas effect on the emission and detection of the backscattered electrons in a VP-SEM at low energy.

The effect of the electron beam skirting on the emission and detection of the backscattered electrons (BSE) in a low vacuum scanning electron microscope is investigated at low energy regime. Monte Carlo computed dependencies of the BSE distribution on the water vapor and air pressure shown a significant increase of the extent of the BSE exit zone. The pressure variation has however a little effect when helium gas is used. A new approach based on the comparison between the sizes of the skirt and the BSE exit zone on the specimen surface provides a useful tool to determine the operating pressure range that ensures minimal degradation of the lateral resolution in BSE imaging mode.

Imaging the Dynamics of Cell Wall Polymer Deposition in the Unicellular Model Plant, Penium margaritaceum.

The unicellular green alga, Penium margaritaceum, represents a novel and valuable model organism for elucidating cell wall dynamics in plants. This organism's cell wall contains several polymers that are highly similar to those found in the primary cell walls of land plants. Penium is easily grown in laboratory culture and is effectively manipulated in various experimental protocols including microplate assays and correlative microscopy. Most importantly, Penium can be live labeled with cell wall-specific antibodies or other probes and returned to culture where specific cell wall developmental events can be monitored. Additionally, live cells can be rapidly cryo-fixed and cell wall surface microarchitecture can be observed with variable pressure scanning electron microscopy. Here, we describe the methodology for maintaining Penium for experimental cell wall enzyme studies.

X-Ray Microanalysis in the Variable Pressure (Environmental) Scanning Electron Microscope.

Electron-excited x-ray microanalysis performed in the variable pressure and environmental scanning electron microscopes is subject to additional artifacts beyond those encountered in the conventional scanning electron microscope. Gas scattering leads to direct contributions to the spectrum from the environmental gas, as well as remote generation of x rays by electrons scattered out of the focussed beam. The analyst can exert some degree of control over these artifacts, but depending on the exact situation, spurious elements can appear at the trace (< 0.01 mass fraction), minor (0.01 mass fraction to 0.1 mass fraction), or even major (> 0.1 mass fraction) levels. Dispersed particle samples give the least compromised results, while fine scale microstructures are the most severely compromised. Procedures to optimize the situation based upon specimen preparation as well as spectral processing are described.