Improvement of Electron Probe Microanalysis of Boron Concentration in Silicate Glasses

The determination of low boron concentrations in silicate glasses by electron probe microanalysis (EPMA) remains a significant challenge. The internal interferences from the diffraction crystal, i.e. the Mo-B4C large d-spacing layered synthetic microstructure crystal, can be thoroughly diminished by using an optimized differential mode of pulse height analysis (PHA). Although potential high-order spectral interferences from Ca, Fe, and Mn on the BKα peak can be significantly reduced by using an optimized differential mode of PHA, a quantitative calibration of the interferences is required to obtain accurate boron concentrations in silicate glasses that contain these elements. Furthermore, the first-order spectral interference from ClL-lines is so strong that they hinder reliable EPMA of boron concentrations in Cl-bearing silicate glasses. Our tests also indicate that, due to the strongly curved background shape on the high-energy side of BKα, an exponential regression is better than linear regression for estimating the on-peak background intensity based on measured off-peak background intensities. We propose that an optimal analytical setting for low boron concentrations in silicate glasses (≥0.2 wt% B2O3) would best involve a proper boron-rich glass standard, a low accelerating voltage, a high beam current, a large beam size, and a differential mode of PHA.

A decade’s worth of otolith PIXE analyses

Over the past 10 years, several thousand otoliths have been analyzed with PIXE (using 2.55 MeV protons) at LIBAF (Lund Ionbeam Analysis Facility, formerly LNMP Lund Nuclear Micro Probe). Over 40 elements have been identified in otoliths, many at levels suitable for PIXE analysis. Readily detectable elements in otoliths starting with Ca are: Ca (the matrix), Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Sr, Y, Zr, Mo, Cd, Sn (difficult), I, Ba (sometimes difficult), Pb (difficult). The detector system, used over this time period, is more sensitive than many other X-ray detector systems, since it consists of eight HPGE detector elements (100 mm2 each), in an annular formation around the beam entrance. Using a thick absorber allows us to use quite high beam current, typically 12 nA, but sometimes up to 20 nA. This permits us to have low detection limits within short analysis times. Additionally, light stable isotope research is widespread in the sciences including ecology. Stable isotopes of N provide information about trophic level (“who eats who”), providing the opportunity to map out the switching of diets from one food type to another. Oxygen isotopes are useful as “environmental thermometers”. Currently, most of such analyses require destruction of the otolith, and nitrogen isotope analysis may require dissolving entire otoliths, thus losing all temporal information. We present new techniques using new types of detectors, double side silicon strip detector (DSSSD). The detectors, electronics and the laboratory setup are described in detail; for our analysis, a MeV proton and a deuterium microbeam at LIBAF is used. The analysis is performed immediately after the PIXE analysis, without moving the sample.

Negative (and very low) thermal expansion in ReO3from 5 to 300 K

This paper reports the accurate measurement of the ReO3cell parameter as a function of temperature. The thermal expansion is confirmed to be negative over most of the temperature range from 5 to 300 K. The main problems with the measurements are the very small variations (in the range of 10−5 Å) in the cell parameter at each temperature, requiring tight control of the stability and reliability of instrumental effects. In particular, achieving monochromator stability over time might be challenging with the high energy and high beam current variations of a third-generation synchrotron facility. On the other hand, such effects are usually checked by the addition of silicon as an internal standard, but the accuracy (and precision) of the published thermal expansion (which is not certified) might not be sufficient for its use when dealing with very small cell parameter variations.