The 50th anniversary of the application of electron probe microanalysis (EPMA) to the Earth Sciences provides an opportunity for an assessment of the state-of-the-art of the technique. Stemming from the introduction of the first automated instruments, the latest developments of EPMA and some typical applications are reviewed with an eye to the future. The most noticeable recent technical achievements such as the field-emission electron gun, the latest generation of energy and wavelength dispersive spectrometers, and the development of analytical methods based on new sets of first principle data obtained by the use of sophisticated computer codes, allow for the extension of the method to the analysis of trace elements, ultra-light elements (down to Li), small particles, and thin films, with a high degree of accuracy and precision and within a considerably reduced volume of interaction. A number of working examples and a thorough list of references provide the reader with a working knowledge of the capabilities and limitations of EPMA today.

One grain, about 100×80 μm in size, occurring in chromitite associated with the layered sequence of the Nurali mafic-ultramafic complex (Southern Urals, Russia) was investigated by electron-microprobe analyses and Raman spectroscopy. The grain is characterized by a spotty, rugged appearance and chemical zoning from which two compositions were calculated: (Pt0.35Pd0.26Fe0.22Cu0.01Ni0.05)0.98O1.02 and (Fe0.90Pt0.58Ni0.28Pd0.13Cu0.08Rh0.01)1.98O1.02. In the lack of X-ray data, Raman spectroscopy established the presence of a diffuse 500–700 band and a sharp peak at 657 cm−1 of relative wavenumber that strongly resemble the Raman spectra of synthetic PtO and PdO (palladinite). It is concluded that the Nurali grain probably represents a platinum group element (PGE) oxide, and does not consist of a mixture of PGE alloys with Fe oxide or hydroxide as reported for other natural PGE-O compounds.

Identification and accurate characterization of platinum-group minerals (PGMs) is usually a very cumbersome procedure due to their small grain size (typically below 10 µm) and inconspicuous appearance under reflected light. A novel strategy for finding PGMs and quantifying their composition was developed. It combines a mineral liberation analyzer (MLA), a point logging system, and electron probe microanalysis (EPMA).

As a first step, the PGMs are identified using the MLA. Grains identified as PGMs are then marked and coordinates recorded and transferred to the EPMA. Case studies illustrate that the combination of MLA, point logging, and EPMA results in the identification of a significantly higher number of PGM grains than reflected light microscopy. Analysis of PGMs by EPMA requires considerable effort due to the often significant overlaps between the X-ray spectra of almost all platinum-group and associated elements. X-ray lines suitable for quantitative analysis need to be carefully selected. As peak overlaps cannot be avoided completely, an offline overlap correction based on weight proportions has been developed. Results obtained with the procedure proposed in this study attain acceptable totals and atomic proportions, indicating that the applied corrections are appropriate.

Electron microprobe analysis of U, Th, and Pb in naturally occurring minerals can indicate their age. Where the Pb is entirely due to the radioactive decay of U and Th, the time since mineral formation or equilibration can be calculated. Uraninite (UO2), monazite (REE PO4), zircon (ZrSiO4), and xenotime (YPO4) have been used, the latter containing U and/or Th in minor proportions. Any stable U- or Th-bearing phase can be considered. Careful analysis is required with attention to interferences, background measurement, detection limits, and Pb-free sample preparation. Extended counting times (600 s) at a probe current >200 nA are recommended. Ages can be determined from uraninite older than 2 Ma for a Pb detection limit of 0.02% and up to 700−1,000 Ma, after which Pb can be lost from the structure. The youngest monazite ages permitted by the Pb detection limit are 50–100 Ma and ages greater than 3,000 Ma have been determined. The method does not provide the detail of isotopic methods, but results can be obtained more readily. Examples show dating of cheralite ((Ca,Ce)(Th,Ce)(PO4)2), a rock containing primary and secondary UO2, and a suite of detrital uraninite grains that formed a part of a mineral exploration program.

Siliciclastic reservoir rocks of the North Alpine Foreland Basin were studied focusing on investigations of pore fillings. Conventional oil and gas production requires certain thresholds of porosity and permeability. These parameters are controlled by the size and shape of grains and diagenetic processes like compaction, dissolution, and precipitation of mineral phases. In an attempt to estimate the impact of these factors, conventional microscopy, high resolution scanning electron microscopy, and wavelength dispersive element mapping were applied. Rock types were established accordingly, considering Poro/Perm data. Reservoir properties in shallow marine Cenomanian sandstones are mainly controlled by the degree of diagenetic calcite precipitation, Turonian rocks are characterized by reduced permeability, even for weakly cemented layers, due to higher matrix content as a result of lower depositional energy. Eocene subarkoses tend to be coarse-grained with minor matrix content as a result of their fluvio-deltaic and coastal deposition. Reservoir quality is therefore controlled by diagenetic clay and minor calcite cementation.Although Eocene rocks are often matrix free, occasionally a clay mineral matrix may be present and influence cementation of pores during early diagenesis. Oligo-/Miocene deep marine rocks exhibit excellent quality in cases when early cement is dissolved and not replaced by secondary calcite, mainly bound to the gas–water contact within hydrocarbon reservoirs.

Optimized quantitative electron-probe microanalysis was applied for compositional characterization of a ferroelectric ceramic single crystal that was made from the complex perovskite-type solid-solution (1–x)Pb(Mg1/3Nb2/3)O3×xPbTiO3 (PMNT). Cation concentrations were determined with high accuracy and ultimate relative experimental uncertainty of ≤±1%, showing that the average chemical composition of the crystal corresponds to Pb(Mg1/3Nb2/3)0.67Ti0.33O3 (i.e., x=0.33), which is close to the morphotropic phase boundary composition. Over the PMNT single crystal slight compositional heterogeneity was measured for concentrations of the perovskite B-site cations Ti4+, Mg2+, and Nb5+, with variations up to ±2.3%, whereas the Pb concentration remained uniform within a variation below ±0.5%.

Using lock-in infrared microscopy as a tool for current detection on the micrometer scale in AC-driven specimens in combination with iterative grinding procedure allows preparation of current dominating microstructure regions on well-polished surfaces. This technique is applied successfully on varistor components based on specially doped ZnO-based varistor ceramics. This peculiar electroceramic material exhibits exceptional high nonlinear current–voltage (I-V) characteristics, described by a power law according I~Vα, caused by double Schottky barriers at the grain boundaries. As a novelty the thermographic response is used to evaluate local electrical properties, namely the nonlinearity coefficient α, on basis of higher order harmonics with respect to the basic electrical driving AC-frequency.

To correlate the observed electrical properties to the microstructure, the polar crystal orientation of the relevant ZnO grains is determined by combining electron backscatter diffraction and orientation-dependent patterns as a result of a chemical etching procedure. These findings support a modified new model for describing the grain boundary controlled current flow in a varistor microstructure including orientation-dependent barrier properties. Hence, the experimentally observed current direction-dependent behavior can be described consistently.

In this paper, the traceability of copper from the anode to the cathode and then the wire rod has been studied in terms of impurity content, microstructure, texture, recrystallization kinetics, and ductility. These characterizations were obtained based on secondary ion mass spectrometry, differential scanning calorimetry (DSC), X-ray diffraction, HV hardness, and electron backscattered diffraction. It is shown that the recrystallization was delayed by the total amount of impurities. From tensile tests performed on cold drawn and subsequently annealed wires for a given time, a simplified model has been developed to link tensile elongation to the chemical composition. This model allowed quantification of the contribution of some additional elements, present in small quantity, on the recrystallization kinetics. The proposed model adjusted for the cold-drawn wires was also validated on both the cathode and wire rod used for the study of traceability.

Several particles of copper accompanied by a few particles of nickel, lead, and a compound composed of selenium containing minor Ni, Si, Cu, and Co were found in human gall, kidney, and bladder stones. The investigated particles occur as tiny grains, <10 µm in size, that are irregularly dispersed in the stones. Therefore, they were studied by scanning electron microscopy and qualitatively analyzed by energy dispersive system. One grain of copper contained a small amount of Ni and Zn, and some grains of nickel proved to contain Cr as trace element. Most of the discovered metals formed a single-phase grain. However, a few grains found in two gallstones were associated with inclusions of calcium and apatite. Based on the results presented in this contribution, we argue that most of the studied metals can be classified as endogenous particles, i.e., directly precipitated from the same fluids that formed their host human stones. This observation suggests that the precipitation and accumulation of metals in some human stones can be considered an efficient way to eliminate them from the human body.

Diluvian Clustering is an unsupervised grid-based clustering algorithm well suited to interpreting large sets of noisy compositional data. The algorithm is notable for its ability to identify clusters that are either compact or diffuse and clusters that have either a large number or a small number of members. Diluvian Clustering is fundamentally different from most algorithms previously applied to cluster compositional data in that its implementation does not depend upon a metric. The algorithm reduces in two-dimensions to a case for which there is an intuitive, real-world parallel. Furthermore, the algorithm has few tunable parameters and these parameters have intuitive interpretations. By eliminating the dependence on an explicit metric, it is possible to derive reasonable clusters with disparate variances like those in real-world compositional data sets. The algorithm is computationally efficient. While the worst case scales as O(N2) most cases are closer to O(N) where N is the number of discrete data points. On a mid-range 2014 vintage computer, a typical 20,000 particle, 30 element data set can be clustered in a fraction of a second.

The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpled discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.

The aim of this paper is to determine the effects of forces exerted on the cantilever probe tip of an atomic force microscope (AFM). These forces vary according to the separation distance between the probe tip and the surface of the sample being examined. Hence, at a distance away from the surface (farther than don), these forces have an attractive nature and are of Van der Waals type, and when the probe tip is situated in the range of a0≤dts≤don, the capillary force is added to the Van der Waals force. At a distance of dts≤a0, the Van der Waals and capillary forces remain constant at intermolecular distances, and the contact repulsive force repels the probe tip from the surface of sample. The capillary force emerges due to the contact of thin water films with a thickness of hc which have accumulated on the sample and probe. Under environmental conditions a layer of water or hydrocarbon often forms between the probe tip and sample. The capillary meniscus can grow until the rate of evaporation equals the rate of condensation. For each of the above forces, different models are presented. The smoothness or roughness of the surfaces and the geometry of the cantilever tip have a significant effect on the modeling of forces applied on the probe tip. Van der Waals and the repulsive forces are considered to be the same in all the simulations, and only the capillary force is altered in order to evaluate the role of this force in the AFM-based modeling. Therefore, in view of the remarkable advantages of the piezoelectric microcantilever and also the extensive applications of the tapping mode, we investigate vibrational motion of the piezoelectric microcantilever in the tapping mode. The cantilever mentioned is entirely covered by two piezoelectric layers that carry out both the actuation of the probe tip and the measuringof its position.

We conducted a semiclassical study on carrier movement in curved graphene. A previous attempt was made to show that curved graphene is a readily available and cheap laboratory material used to study general relativity effects, especially if the electron energies satisfy ${\rm 4}\:\mu {\rm eV}\,\ll\,\left| E \right|\,\ll\,{\rm 3}\:{\rm eV}$ . Furthermore, a gravitational-like lens can be constructed based on a special graphene ripple; this lens has neither chromatic nor cometic aberration. One can design an ideal electron lens using a graphene ripple.

Short illumination wavelength allows an extension of the diffraction limit toward nanometer scale; thus, improving spatial resolution in optical systems. Soft X-ray (SXR) radiation, from “water window” spectral range, λ=2.3–4.4 nm wavelength, which is particularly suitable for biological imaging due to natural optical contrast provides better spatial resolution than one obtained with visible light microscopes. The high contrast in the “water window” is obtained because of selective radiation absorption by carbon and water, which are constituents of the biological samples. The development of SXR microscopes permits the visualization of features on the nanometer scale, but often with a tradeoff, which can be seen between the exposure time and the size and complexity of the microscopes. Thus, herein, we present a desk-top system, which overcomes the already mentioned limitations and is capable of resolving 60 nm features with very short exposure time. Even though the system is in its initial stage of development, we present different applications of the system for biology and nanotechnology. Construction of the microscope with recently acquired images of various samples will be presented and discussed. Such a high resolution imaging system represents an interesting solution for biomedical, material science, and nanotechnology applications.

Atomic force microscopy (AFM) and other forms of scanning probe microscopy have been successfully used to assess biomechanical and bioelectrical characteristics of individual cells. When extending such approaches to heterogeneous tissue, there exists the added challenge of traversing the tissue while directing the probe to the exact location of the targeted biological components under study. Such maneuvers are extremely challenging owing to the relatively small field of view, limited availability of reliable visual cues, and lack of context. In this study we designed a system that leverages the visual topology of the serial tissue sections of interest to help guide robotic control of the AFM stage to provide the requisite navigational support. The process begins by mapping the whole-slide image of a stained specimen with a well-matched, consecutive section of unstained section of tissue in a piecewise fashion. The morphological characteristics and localization of any biomarkers in the stained section can be used to position the AFM probe in the unstained tissue at regions of interest where the AFM measurements are acquired. This general approach can be utilized in various forms of microscopy for navigation assistance in tissue specimens.

Two polyoxometalates (POMs), synthesized through a self-assembling method, were used in the treatment of streptozotocin (STZ)-induced diabetic rats. One of these nanocompounds [tris(vanadyl)-substituted tungsto-antimonate(III)-anions—POM1] was previously described in the literature, whereas the second [tris-butyltin-21-tungsto-9-antimonate(III)-anions—POM2], was prepared by us based on our original formula. In rats with STZ-induced diabetes treated with POMs (up to a cumulative dose of 4 mg/kg bodyweight at the end of the treatments), statistically significant reduced levels of blood glucose were measured after 3 weeks, as compared with the diabetic control groups (DCGs). Ultrastructural analysis of pancreatic β-cells (including the mean diameter of secretory vesicles and of their insulin granules) in the treated diabetic rats proved the POMs contribute to limitation of cellular degeneration triggered by STZ, as well as to the presence of increased amounts of insulin-containing vesicles as compared with the DCG. The two POMs also showed hepatoprotective properties when ultrastructural aspects of hepatocytes in the experimental groups of rats were studied. Based on our in vivo studies, we concluded that the two POMs tested achieved hypoglycemiant effects by preventing STZ-triggered apoptosis of pancreatic β-cells and stimulation of insulin synthesis.

The aim of the present study was to isolate human mesenchymal stem cells (MSCs) from palatal connective and periodontal granulation tissues and to comparatively evaluate their properties. MSCs were isolated using the explant culture method. Adherence to plastic, specific antigen makeup, multipotent differentiation potential, functionality, and ultrastructural characteristics were investigated. The frequency of colony-forming unit fibroblasts for palatal-derived mesenchymal stem cells (pMSCs) was significantly higher than that of granulation tissue-derived mesenchymal stem cells (gtMSCs). A significantly higher population doubling time and lower migration potential were recorded for gtMSCs than for pMSCs. Both cell lines were positive for CD105, CD73, CD90, CD44, and CD49f, and negative for CD34, CD45, and HLA-DR, but the level of expression was different. MSCs from both sources were relatively uniform in their ultrastructure. Generally, both cell lines possessed a large, irregular-shaped euchromatic nucleus, and cytoplasm rich in mitochondria, lysosomes, and endoplasmic reticulum. The periphery of the plasma membrane displayed many small filopodia. MSCs from both cell lines were successfully differentiated into osteogenic, adiopogenic, and chondrogenic lineages. Both healthy and diseased tissues may be considered as valuable sources of MSCs for regenerative medicine owing to the high acceptance and fewer complications during harvesting.

The inflammatory resorption of dental root apex (i.e., the process of removal of cementum and/or dentine through the activity of resorbing cells) may show different configurations and damage the apical root structure. As knowing the morphology of resorption areas of human teeth is essential for the success of endodontic treatments, we investigated the apical resorption by scanning electron microscopy, focusing on roots with granulomas. A total of 30 teeth (with penetrating carious lesions and chronic periapical lesions) were examined, the apical third of the roots were removed and analyzed to estimate periforaminal and foraminal resorption, shape and morphology of foramen resorption, centering of the periforaminal resorption area, and diameters of each apical foramen. Periforaminal resorption was present in all samples, whereas foraminal resorption was present in 92% of cases (mainly funnel shaped). Lacunae were observed in the foraminal resorption area with an average diameter of 35±14 μm. The major and minor diameters of the foramina in teeth with resorption were 443 and 313 μm, respectively (higher than in healthy teeth). This result indicates an expansion of the apical diameters caused by the pathology, which could encourage a different clinical instrumentation for these teeth.

The aim of interfacial nanoleakage evaluation is to gain a better understanding of degradation of the adhesive–dentin interface. The acid–base resistant zone (ABRZ) is recognized at the bonded interface under the hybrid layer (HL) in self-etch adhesive systems after an acid–base challenge. The purpose of this study was to evaluate nanoleakage in HL and ABRZ using three self-etch adhesives; Clearfil SE Bond (SEB), Clearfil SE One (SEO), and G-Bond Plus (GBP). One of the three adhesives was applied on the ground dentin surface and light cured. The specimens were longitudinally divided into two halves. One half remained as the control group. The others were immersed in ammoniacal silver nitrate solution, followed by photo developing solution under fluorescent light. Following this, the specimens were subjected to acid–base challenges with an artificial demineralization solution (pH4.5) and sodium hypochlorite, and prepared in accordance with common procedures for transmission electron microscopy (TEM) examination. The TEM images revealed silver depositions in HL and ABRZ due to nanoleakage in all the adhesives; however, the extent of nanoleakage was material dependent. Funnel-shaped erosion beneath the ABRZ was observed only in the all-in-one adhesive systems; SEO and GBP, but not in the two-step self-etch adhesive system; SEB.