Multivariate statistical analyses of geochemical, mineralogical, and cation-exchange capacity (CEC) data from a Venezuelan oil well were used to construct a model which relates elemental concentrations to mineral abundances. An r-mode factor analysis showed that most of the variance could be accounted for by four independent factors and that these factors were related to individual mineral components: kaolinite, illite, K-feldspar, and heavy minerals. Concentrations of Al, Fe, and K in core samples were used to estimate the abundances of kaolinite, illite, K-feldspar, and, by subtraction from unity, quartz. Concentrations of these elements were also measured remotely in the well by geochemical logging tools and were used to estimate these mineral abundances on a continuous basis as a function of depth. The CEC was estimated from a linear combination of the derived kaolinite and illite abundances. The formation's thermal neutron capture cross section estimated from the log-derived mineralogy and a porosity log agreed well with the measured data. Concentrations of V, among other trace elements, were modeled as linear combinations of the clay mineral abundances. The measured core V agreed with the derived values in shales and water-bearing sands, but exceeded the clay-derived values in samples containing heavy oil. The excess V was used to estimate the V content and API Gravity of the oil. The log-derived clay mineralogy was used to help distinguish nonmarine from transitional depositional environments. Kaolinite was the dominant clay in nonmarine deposits, whereas transitional sediments contained more illite.

Electron-excited X-ray microanalysis with energy-dispersive spectrometry (EDS) proceeds through the application of the software that extracts characteristic X-ray intensities and performs corrections for the physics of electron and X-ray interactions with matter to achieve quantitative elemental analysis. NIST DTSA-II is an open-access, fully documented, and freely available comprehensive software platform for EDS quantification, measurement optimization, and spectrum simulation. Spectrum simulation with DTSA-II enables the prediction of the EDS spectrum from any target composition for a specified electron dose and for the solid angle and window parameters of the EDS spectrometer. Comparing the absolute intensities for measured and simulated spectra reveals correspondence within ±25% relative to K-shell and L-shell characteristic X-ray peaks in the range of 1–11 keV. The predicted M-shell intensity exceeds the measured value by a factor of 1.4–2.2 in the range 1–3 keV. The X-ray continuum (bremsstrahlung) generally agrees within ±10% over the range of 1–10 keV. Simulated EDS spectra are useful for developing an analytical strategy for challenging problems such as estimating trace detection levels.

In insects, the number, cytological and histological structures, and the spherocrystals of the Malpighian tubules (MTs) can vary considerably in different insect groups. These differences are considered important because they can be used as taxonomic characters. For this purpose, the ultrastructure of the MT epithelial cells in Leptophyes albovittata (Kollar, 1833) (Orthoptera, Tettigoniidae) was examined by light microscopy, scanning electron microscopy, and transmission electron microscopy. The wall of each tubule consists of a single layer of cells. These cells have round-shaped nuclei. Two different cell types were demonstrated in the tubule cell. These are cells that have electron-dense cytoplasm and electron-lucent cytoplasm. It was observed that the cytoplasm of these cells has many spherocrystals. The chemical composition of the spherocrystals was found to be high in carbon, phosphorus, and manganese in tubule cells.

Auger spectroscopy has not found widespread application in the geological sciences, largely because specimens are often non-conductors that charge under electron beams. However, it has proven to be useful for the characterization of sub-micrometer mineral grains in certain meteorites, where sample charging issues can be mitigated. We describe the development of analytical protocols for the measurement of presolar silicate grains using Auger spectroscopy and review how this technique has helped our understanding of the stellar origin and subsequent evolution of these grains.

The discovery of the Nan'ao One shipwreck off the southern coast of China throws new light onto Chinese maritime trade during the late Ming period. The primary cargo was a massive consignment of blue-and-white export porcelain, most probably destined for markets in Southeast Asia or Europe. Compositional analysis was performed on 11 fragments of blue-and-white export porcelain from the wreck site and on 64 samples from 3 Chinese porcelain production centres. The results indicate that the blue-and-white export porcelain recovered from the Nan'ao One came from two sources: the Jingdezhen and Zhangzhou kilns. Given the location of the shipwreck, the most probable destinations were the Portuguese trading centre at Macau or the Dutch at Batavia.

A simple model is proposed to account for the loss of collected X-ray signal by the shadowing of X-ray detectors in the scanning transmission electron microscope. The model is intended to aid the analysis of three-dimensional elemental data sets acquired using energy-dispersive X-ray tomography methods where shadow-free specimen holders are unsuitable or unavailable. The model also provides a useful measure of the detection system geometry.

The Proterozoic carbonate stromatolites of the Pahrump Group from the Crystal Spring formation exhibit interesting layering patterns. In continuous vertical formations, there are sections of chevron-shaped stromatolites alternating with sections of simple horizontal layering. This apparent cycle of stromatolite formation and lack of formation repeats several times over a vertical distance of at least 30 m at the locality investigated. Small representative samples from each layer were taken and analysed using X-ray diffraction (XRD), X-ray fluorescence (XRF), environmental scanning electron microscopy – energy dispersive X-ray spectrometry, and were optically analysed in thin section. Optical and spectroscopic analyses of stromatolite and of non-stromatolite samples were undertaken with the objective of determining the differences between them. Elemental analysis of samples from within each of the four stromatolite layers and the four intervening layers shows that the two types of layers are chemically and mineralogically distinct. In the layers that contain stromatolites the Ca/Si ratio is high; in layers without stromatolites the Ca/Si ratio is low. In the high Si layers, both K and Al are positively correlated with the presence and levels of Si. This, together with XRD analysis, suggested a high K-feldspar (microcline) content in the non-stromatolitic layers. This variation between these two types of rocks could be due to changes in biological growth rates in an otherwise uniform environment or variations in detrital influx and the resultant impact on biology. The current analysis does not allow us to choose between these two alternatives. A Mars rover would have adequate resolution to image these structures and instrumentation capable of conducting a similar elemental analysis.

Interest in atmospheric aerosol issues has been increasing worldwide. X-ray fluorescence (XRF) is an important atmospheric aerosol monitoring tool for inorganic component analysis, because XRF is a rapid and easy analysis method. In particular, Energy dispersive X-ray fluorescence (EDXRF) has drawn attention for aerosol analysis. However, EDXRF has difficulties that: (1) many overlapping peaks exist for aerosol filter analysis and (2) many thin-film standard samples are required when an empirical calibration method is employed. Accurate analysis method of aerosol filter samples without the need for large sets of standards by semi-quantitative analysis software RPF–SQX (Rigaku profile fitting–spectra quant X), which includes the exact profile fitting and thin-film fundamental parameter (FP) method, is described using the EDXRF spectrometer equipped with secondary targets and polarized optics.

Elemental analysis of dental hard tissues is of importance. The aim of this study is to evaluate X-ray microanalysis (XRMA) of bovine enamel in a scanning electron microscope (SEM) with different coatings. The buccal surface of bovine incisors was polished flat, one-third was coated with carbon, one-third with gold, leaving one-third uncoated for XRMA in an SEM equipped with an energy-dispersive microanalysis system. The elements oxygen, sodium, magnesium, phosphorous, chlorine, potassium, and calcium were analyzed using their respective characteristic K X-ray series. Comparisons were made with analyses of glass produced by fusion of the bovine enamel, showing that oxygen analyses using the K X-ray series are reliable and preferable to calculating oxygen by stoichiometry for natural enamel. For the gold-coated and uncoated analyses, carbon was also measured using the K X-ray series. Small area Analyses in small areas (80 × 80 μm) in variable pressure-SEM mode with low vacuum (20 Pa), without any coating, midway between 40 μm wide gold lines 140 μm apart to avoid build-up of electrostatic charge is the preferred method, especially if carbon is included in the analysis. The analyses of bovine enamel are sufficiently reproducible to be regarded as quantitative for all elements except carbon.

Electron Rutherford backscattering (ERBS) is a new technique that could be developed into a tool for materials analysis. Here we try to establish a methodology for the use of ERBS for materials analysis of more complex samples using bone minerals as a test case. For this purpose, we also studied several reference samples containing Ca: calcium carbonate (CaCO3) and hydroxyapatite and mouse bone powder. A very good understanding of the spectra of CaCO3 and hydroxyapatite was obtained. Quantitative interpretation of the bone spectrum is more challenging. A good fit of these spectra is only obtained with the same peak widths as used for the hydroxyapatite sample, if one allows for the presence of impurity atoms with a mass close to that of Na and Mg. Our conclusion is that a meaningful interpretation of spectra of more complex samples in terms of composition is indeed possible, but only if widths of the peaks contributing to the spectra are known. Knowledge of the peak widths can either be developed by the study of reference samples (as was done here) or potentially be derived from theory.

Because of its great potential to provide data on contacts and overseas trade, ivory has aroused a great deal of interest since the very start of research into Iberian late prehistory. Research recently undertaken by the German Archaeological Institute in Madrid in collaboration with a number of other institutions has provided valuable contributions to the study of ivory in the Iberian Copper Age and Early Bronze Age. One of the archaeological sites that is contributing the most data for analysing ivory from the Copper Age in southern Iberia is Valencina de la Concepción (Seville), which is currently the focus of several debates on the development of social complexity. This article contributes to this line of research by providing new, unpublished evidence and by examining the significance of ivory craftsmanship in commercial, social, and ideological terms. It also assesses in greater detail the prominent part played by luxury ivory items as an expression of social status and power.

Methods using X-ray fluorescence have been developed to identify cometary material captured in aerogel during the NASA Stardust mission to Comet 81P/Wild 2. These analytical methods are necessitated by the levels of trace contaminants present in the aerogel. The cometary material disaggregates during deceleration in the aerogel, so fluorescence mapping of the entire track (which can be several millimeters long) is necessary. Distinguishing those pixels which have cometary material and aerogel from those which have only cometary material can be very challenging. We have chosen a “dual threshold” method, with some pixels clearly having only aerogel (plus contaminants) and other pixels clearly having cometary and aerogel material. Between these two threshold levels is a set of pixels which cannot be easily ascribed to one or the other. By leaving these pixels out of the analysis, the estimate of cometary material is improved.

Persistence of gunshot residue (GSR) simultaneously collected from hands, face and hair, and clothing of the shooting person was examined. Samples were collected from five shooters in nine time intervals after a single shoot with a Luger 9 mm pistol, in the range of 0–4 h and examined with scanning electron microscopy and energy dispersive X-ray spectrometry. Numbers of particles, frequencies of occurrence of certain compositions of particles, and their sizes in function of the time intervals were inspected. The greatest numbers of particles were observed in samples collected from hands right after shooting, but they decrease quickly with time. In samples collected from the face smaller initial numbers of particles were found, but they lasted at a similar level longer. The estimated half-life times of particles were less than 1 h for samples taken from the hands, over 1 h for clothing and about 2–3 h for the face. In samples collected at longer intervals after shooting, there were particles present of small sizes and irregular shapes. The results demonstrate that including evidence collected from the suspect's face and hair may increase the probability of detection of GSR in cases when the suspect has not been apprehended immediately after the investigated incident.

A radioactive particle embedded in a sediment collected from the Irish Sea was examined with spectrometric methods to understand the potential bioavailability of its constituents. Images of the particle surface were acquired in the backscattering mode by scanning electron microscopy. The elemental composition of the particle surface layer was measured using energy dispersive (SEM-EDX) and wavelength dispersive (SEM-WDX) X-ray spectrometers. The investigation showed that the sample consists of a calcite matrix in which uranium is present in the form of separate inclusions. The diameter of U inclusions was less than 10 μm. Synchrotron radiation based X-ray fluorescence in confocal geometry (confocal μ-XRF) was used to determine the spatial distribution of elements in the particle. Three-dimensional reconstructions of the Ca, Cr, Mn, Fe, Zn, Sr, Ba, Pb, and U distributions were performed. The oxidation state of uranium in the different inclusions was determined by synchrotron radiation based X-ray absorption in confocal geometry (confocal μ-XANES). The isotopic composition of uranium was measured by secondary ion mass spectrometry. The results revealed that uranium was depleted in 235U. Pu and other actinides were not detected.