Nephelometric (light scattering) methods for the determination of Ca and Ba in the 0–30 ppm range, and their application to the estimation of the cation exchange capacity (±10%) of small (≤30 mg) samples of clay minerals, are described and evaluated.

Maternal depression and anxiety are associated with infant and mother self- and interactive difficulties. Although maternal depression and anxiety usually co-occur, studies taking this comorbidity into account are few. Despite some literature, we lack a detailed understanding of how maternal depressive and anxiety symptoms may be associated with patterns of mother–infant interaction. We examined associations of maternal postpartum depressive and anxiety symptoms with infant and mother self- and interactive patterns by conducting multi-level time-series models in a sample of 56 Turkish mothers and their 4-month infants. Time-series models assessed the temporal dynamics of interaction via infant and mother self- and interactive contingency. Videotaped face-to-face interaction was coded on a 1s time base for infant and mother gaze and facial affect, infant vocal affect, and mother touch. Results indicated that mothers with high depressive symptoms were vulnerable to infants looking away, reacting with negative touch; their infants remained affectively midrange, metaphorically distancing themselves from mothers’ affect. Mothers with high anxiety symptoms were vulnerable to infants becoming facially dampened and mothers reacted with negative facial affect. Altered infant and mother self-contingency patterns were largely opposite for maternal depressive and anxiety symptoms. These patterns describe foundational processes by which maternal postpartum mood is transmitted to the infant and which may affect infant development.

Because the essential quality metrics of blast furnace slag are based on its oxide composition, the determination of chemical compositions of unhydrated slag grains in an aged concrete could be useful for understanding its past performance and in predicting the remaining service life of existing slag-bearing concrete. In this research, the authors explored the feasibility of using standard-based energy-dispersive X-ray spectroscopy (EDS) microanalysis, in tandem with electron imaging, as a tool for quantitative measurement of the chemical composition of blast furnace slag grains in cement/concrete. In the experimental study, seven concrete samples representing various service life durations were collected in the Netherlands. The microanalysis results of the samples revealed that the change in slag chemistry is insignificant for samples B (1985) to F (2006); however, elevated CaO and SiO2 contents are found in slag used for sample G (2015), opposite to that of Al2O3 and MgO. After discussing compositional characterization, the paper discusses favorable microanalysis protocols for acceptable elemental quantification accuracy. It was concluded that quantitative EDS microanalysis is a strong tool to characterize the chemical composition of unhydrated slag used in field concrete, which could potentially contribute to understanding the correlations between composition and long-term performance in slag concrete structures.

Recent years have seen increased crossover of microscopy techniques developed for transmission electron microscopes (TEMs) being utilized as well in scanning electron microscopes (SEMs). The order of magnitude lower beam energies available in SEMs correspond with significantly different beam-sample interactions that must be accounted for when examining freestanding films. This is especially important for composition analysis via energy dispersive X-ray spectroscopy (EDS) since lower-energy transmission experiments mean X-ray volumes become comparable to sample dimensions. To better understand this scenario, we report results of an SEM-EDS study of terraced freestanding films comprising binary compounds with well-defined atomic ratios. Guided by Monte Carlo simulations, EDS line scan data were collected at different beam energies across segments of varying thicknesses. The results of quantification analysis using different models are compared for multiple combinations of beam energy, sample thickness, and material density, from which some general guidelines are provided for SEM-EDS analysis of freestanding films.

Hyperspectral soft X-ray emission (SXE) and cathodoluminescence (CL) spectrometry have been used to investigate a carbonaceous-rich geological deposit to understand the crystallinity and morphology of the carbon and the associated quartz. Panchromatic CL maps show both the growth of the quartz and the evidence of recrystallization. A fitted CL map reveals the distribution of Ti4+ within the grains and shows subtle growth zoning, together with radiation halos from 238U decay. The sensitivity of the SXE spectrometer to carbon, together with the anisotropic X-ray emission from highly orientated pyrolytic graphite, has enabled the C Kα peak shape to be used to measure the crystal orientation of individual graphite regions. Mapping has revealed that most grains are predominantly of a single orientation, and a number of graphite grains have been investigated to demonstrate the application of this new SXE technique. A peak fitting approach to analyzing the SXE spectra was developed to project the C Kα 2pz and 2p(x+y) orbital components of the graphite. The shape of these two end-member components is comparable to those produced by electron density of states calculations. The angular sensitivity of the SXE spectrometer has been shown to be comparable to that of electron backscatter diffraction.

The aim of the present study was to map the painting materials, degradation processes, and biological features present on the mural painting in the church of St. Mary in Beram (Croatia) to study their possible interaction and produce information helping the preservation of this valuable painting. The research was conducted on micro samples of painting materials taken from different sites along the painting and the characterization of the present fungal species was carried out. The painting samples, together with observable patinas and degradation products, were studied by optical microscopy (OM), scanning electron microscopy, energy-dispersive spectroscopy (SEM/EDS), Fourier-Transform Infrared spectroscopy, and powder X-ray diffraction. Fungal diversity was studied using cultivation methods followed by OM and SEM analyses in addition to molecular analysis. The results contribute to the characterization of the original painting materials, successively added materials and occurred interventions, to the understanding of degradation progressions and fungal biotransformation processes. A mineral, cumengite, a copper-based pigment extremely rarely used in art, was found. Its occurrence together with barium sulfate, gypsum, and calcium oxalate possibly produced by microbiological activity was studied and information was added regarding the composition of painting materials in St. Mary church mural cycle.

A new program has been established by the Microscopy Society of America (MSA) to provide funding for bold, new, strategic initiatives that further the goals of the Microscopy Society of America and the fields of microscopy, microanalysis, and imaging in general. Three bold, new initiatives won initial funding for 2019: a proposal to fund an international micrograph competition, an initiative to set up an MSA Student Council web presence to host web events targeted to microscopy students and developing professionals, and a plan to provide a uniform template and hosting service for MSA Local Affiliated Societies.

The detailed kinetics study of erythrocyte deformability is useful for the early diagnosis of blood diseases and for monitoring the blood rheology. Present solutions for a three-dimensional (3D) reconstruction of erythrocytes has a limited potential. This study aimed to use erythrocyte transmission electron images (ETIs) to evaluate the morphological relationship between adjacent ETIs and generate erythrocytes 3D model. First, ultrathin serial sections of skeletal muscle tissue were obtained using an ultramicrotome. Further, the set of ETIs in a capillary were captured by transmission electron microscopy. The images were aligned by translations and rotations using custom software to optimize the morphological relationship between adjacent ETIs. These coordinate transformations exploit the unique principal axis of inertia of each image to define the body coordinate system and hence provide the means to accurately reconnect the adjacent ETIs. The sum of the distances between the corresponding points on the boundary of adjacent ETIs was minimized and, further, was optimized by using physiological relationship between the adjacent ETIs. The analysis allowed to define precise virtual relationship between the adjacent erythrocytes. Finally, extracted erythrocytes’ cross-section images allowed to generate 3D model of the erythrocytes.

The ICDD has developed a microanalysis tool to help scientists identify minerals from their elemental analyses, most typically micro-XRF or a microprobe analysis. Many minerals have characteristic elemental profiles that can often distinguish the mineral from others by their composition differences. In Release 2016 ICDD® PDF-4 databases 20 670 unique compositions have been identified out of 45 497 mineral and mineral-related entries. The application utilizes several common features of PDF® databases to enhance correct identification, most notably those formulas are expressed in weight and atomic percent, data sets are classified by mineral nomenclature and structural classifications, and most minerals have associated atomic and molecular structures. These crystal structures are very useful in determining compositional variants and solid solutions. The ICDD has developed algorithms that are analogous to the search/match processes used for powder diffraction identification. Data can be input as either the element or common oxide. To test the algorithm and graphics interfaces we compared results from the microanalysis module to published data from the Smithsonian Microbeam reference mineral collection. The software correctly identified 24/28 minerals by the highest merit score in the algorithm. In two cases, an isoelemental mineral was identified and in two other cases, the specimens had more elements than the reference standards hindering positive phase identification.

By using an experimental model of dexamethasone-induced osteoporosis we investigated the effects of different therapeutic schemes combining sodium alendronate (SA) and simvastatin on bone mineral and protein composition, microstructural and mechanical remodeling. Wistar rats were randomized into eight groups: G1: non-osteoporotic; G2: osteoporotic; G3, G4, and G5: osteoporotic+SA (0.2, 0.4, and 0.8 mg/kg, respectively); G6, G7, and G8: osteoporotic+SA (0.2, 0.4, and 0.8 mg/kg, respectively)+simvastatin (0.4, 0.6, and 1 mg/kg, respectively). Osteoporosis was induced by dexamethasone (7 mg/kg, i.m.) once a week for 5 weeks. All treatments were administered for 8 weeks. Dexamethasone increased serum levels of alkaline phosphatase, calcium, phosphorus, and urea, especially in non-treated animals, which showed severe osteoporosis. Dexamethasone also induced bone microstructural fragility and reduced mechanical resistance, which were associated with a marked depletion in mineral mass, collagenous and non-collagenous protein levels in cortical and cancellous bone. Although SA has attenuated osteoporosis severity, the effectiveness of drug therapy was enhanced combining alendronate and simvastatin. The restoration in serum parameters, organic and inorganic bone mass, and mechanical behavior showed a dose-dependent effect that was potentially related to the complementary mechanisms by which each drug acts to induce bone anabolism, accelerating tissue repair.

Scanning electron microscopy with energy-dispersive spectrometry has been applied to the analysis of various materials at low-incident beam energies, E0≤5 keV, using peak fitting and following the measured standards/matrix corrections protocol embedded in the National Institute of Standards and Technology Desktop Spectrum Analyzer-II analytical software engine. Low beam energy analysis provides improved spatial resolution laterally and in-depth. The lower beam energy restricts the atomic shells that can be ionized, reducing the number of X-ray peak families available to the analyst. At E0=5 keV, all elements of the periodic table except H and He can be measured. As the beam energy is reduced below 5 keV, elements become inaccessible due to lack of excitation of useful characteristic X-ray peaks. The shallow sampling depth of low beam energy microanalysis makes the technique more sensitive to surface compositional modification due to formation of oxides and other reaction layers. Accurate and precise analysis is possible with the use of appropriate standards and by accumulating high count spectra of unknowns and standards (>1 million counts integrated from 0.1 keV to E0).

The aim of the present work was to investigate birefringence and morphology of the secretory-stage enamel organic extracellular matrix (EOECM), and structural and mechanical properties of mature enamel of upper incisors from adult rats that had been treated with pamidronate disodium (0.5 mg/kg/week for 56 days), using transmitted polarizing and bright-field light microscopies (TPLM and BFLM), energy-dispersive X-ray (EDX) analysis, scanning electron microscopy (SEM) and microhardness testing. BFLM showed no morphological changes of the EOECM in pamidronate and control groups, but TPLM revealed a statistically significant reduction in optical retardation values of birefringence brightness of pamidronate-treated rats when compared with control animals (p<0.01). EDX analysis showed that pamidronate-induced statistically significant decrease in phosphorus’ quantity in outer mature enamel (p<0.01) and an increase in the calcium/phosphorus ratio in that structure (p<0.05). Pamidronate did not induce ultra-structural alterations in mature enamel as revealed by SEM and did not cause a reduction in its microhardness (p>0.05). The present study indicates that pamidronate can affect birefringence of the secretory-stage EOECM, which does not seem to be associated with significant changes in morphological and/or mechanical properties of mature enamel.

This paper reports an unusual green pigment, brochantite (Cu4(SO4)(OH)6), on 16th-century Portuguese-Flemish paintings, attributed to the Master Frei Carlos workshop. This green mineral is usually identified as an impurity or alteration product in the green pigments verdigris (Cu(CH3COO)2nCu(OH)2) or malachite (CuCO3 Cu(OH)2). However, after thorough investigation with a broad range of analytical techniques, it became clear that, in this case, brochantite was applied as a pigment. The abundance, pigment granulometry, and pigment morphology suggest intentional use by this Portuguese-Flemish Master as a natural pigment rather than its accidental use as an alteration product. This seems to be a distinguishable feature to other painters (Flemish and Portuguese) working in Portugal at the beginning of the 16th century.

The multi-analytical study of these easel paintings was first performed by physical imaging techniques and material characterization was carried out by optical microscopy, micro-Fourier-transform infrared-spectroscopy, micro-Raman spectroscopy, scanning electron microscopy coupled with energy dispersive X-ray spectrometry, and micro-X-ray diffraction analysis (XRD).

Closed form analytical equations used to calculate the collection solid angle of six common geometries of solid-state X-ray detectors in scanning and scanning/transmission analytical electron microscopy are presented. Using these formulae one can make realistic comparisons of the merits of the different detector geometries in modern electron column instruments. This work updates earlier formulations and adds new detector configurations.

The use of analytical spectroscopies during scanning/transmission electron microscope (S/TEM) investigations of micro- and nano-scale structures has become a routine technique in the arsenal of tools available to today’s materials researchers. Essential to implementation and successful application of spectroscopy to characterization is the integration of numerous technologies, which include electron optics, specimen holders, and associated detectors. While this combination has been achieved in many instrument configurations, the integration of X-ray energy-dispersive spectroscopy and in situ liquid environmental cells in the S/TEM has to date been elusive. In this work we present the successful incorporation/modifications to a system that achieves this functionality for analytical electron microscopy.

Organic matter (OM) entrapped in calcite is regularly used for environmental studies; however, insertion mechanisms and types of interaction remain poorly understood. The present study used a new methodology to investigate interactions between OM and the calcite matrix during crystallization processes with humic acid (HA) entrapment. A multimethod approach confirmed that HA is both adsorbed onto the calcite surface and incorporated into the calcite lattice during crystallization. Our results also confirm the log-linear correlation between fluorescence intensity and calcite matrix HA concentration. Fourier transform infrared spectroscopy showed that HA in colloidal conformation is adsorbed onto the calcite surface as a result of the structure of the OH stretching band. We also developed a new method based on synchrotron analysis that uses sulfur as a tracer element for entrapped HA and that localizes the OM electrostatically adsorbed onto the calcite surface. Changes in the sulfur environment, determined using X-ray absorption near-edge structure spectroscopy, indicated more complex insertion mechanisms than simple adsorption of HA during calcite crystallization. Desorption experiments revealed the stability of the OM atomic structure and its layered nature. These results allowed us to draw up a general model of OM insertion in calcite.

The measurement of near-infrared (NIR) cathodoluminescence (CL) with sufficient sensitivity to allow full spectral mapping has been investigated through the application of optimized grating spectrometers that allow the ultraviolet (UV), visible, and NIR CL spectra to be measured simultaneously. Two optical spectrometers have been integrated into an electron microprobe, allowing simultaneous collection of hyperspectral CL (UV-NIR), characteristic X-rays, and electron signals. Combined hyperspectral CL spectra collected from two natural apatite (Ca5[PO4]3[OH,F]) samples from Wilberforce (Ontario, Canada) and Durango (Mexico) were qualitatively analyzed to identify the emission centers and then deconvoluted pixel-by-pixel using least-squares fitting to produce a series of ion-resolved CL intensity maps. Preliminary investigation of apatite has shown strong NIR emissions associated primarily with the rare-earth element Nd. Details of growth and alteration were revealed in the NIR that were not discernable with electron-induced X-ray mapping. Intense emission centers from Nd3+ and Sm3+ were observed in the spectra from both apatites, along with minor emissions from other 3+ rare-earth elements. Quantitative electron probe microanalysis was performed on points within the mapped area of the Durango apatite to produce a calibration line relating cathodoluminescent intensity of the fitted peak centered at 1,073 nm (1.156 eV) to the Nd concentration.

BaFCl:Sm3+ is an efficient photoluminescent storage phosphor for ionizing radiation. Cathodoluminescence (CL) microanalysis enables the Sm2+ and Sm3+ oxidation states of samarium doped BaFCl to be easily identified, provides information about electron-beam and X-ray induced modification of BaFCl:Sm, and enables the synthesis dependent spatial distribution of samarium dopants of <100 ppm concentration to be determined with sub-100 nm resolution at 295 K. CL spectroscopy of BaFCl:Sm particles reveals broad CL emissions at ∼360 and ∼500 nm associated with Vk(Cl−) and oxygen-vacancy defects in the BaFCl host lattice and fine structure CL emissions associated with major 4GJ → 6HJ (Sm3+) and 5DJ → 7FJ (Sm2+) transitions. CL microanalysis shows samarium dopants are uniformly distributed in conventional sintered microcrystalline BaFCl:Sm. In contrast, CL investigations reveal that for BaFCl:Sm nanoparticles, which have been prepared using a co-precipitation method, with greatly improved Sm3+ → Sm2+ conversion efficiency, the samarium dopants are concentrated near the particle surface resulting in a BaFCl:Sm3+ shell surrounding the BaFCl core, which is stable to energetic irradiation.

Aluminum-lithium alloys are widespread in the aerospace industry. The new 2099 and 2199 alloys provide improved properties, but their microstructure and texture are not well known. This article describes how state-of-the-art field-emission scanning electron microscopy (FE-SEM) can contribute to the characterization of the 2099 aluminum-lithium alloy and metallic alloys in general. Investigations were carried out on bulk and thinned samples. Backscattered electron imaging at 3 kV and scanning transmission electron microscope imaging at 30 kV along with highly efficient microanalysis permitted correlation of experimental and expected structures. Although our results confirm previous studies, this work points out possible substitutions of Mg and Zn with Li, Al, and Cu in the T1 precipitates. Zinc and magnesium are also present in “rice grain”–shaped precipitates at the grain boundaries. The versatility of the FE-SEM is highlighted as it provides information in the macro- and microscales with relevant details. Its ability to probe the distribution of precipitates from nano- to microsizes throughout the matrix makes FE-SEM an essential technique for the characterization of metallic alloys.