Direct analysis of Al2O3 powders by total reflection X-ray fluorescence spectrometry
A direct analysis procedure for the determination of trace impurities of Ca, V, Cr, Mn, Fe, Ni, Cu, Zn and Ga in Al2O3 ceramic powders by total reflection X-ray fluorescence spectrometry (TXRF) is described. The powders were analysed in the form of slurries containing 1–10 mg mL−1 of powder. The use of the procedure in the case of powders with differing grain size and for different slurry concentrations was investigated. Three different quantification possibilities were compared, namely the use of Al as a matrix component, the use of Fe as a trace element contained in the sample or of Co added in concentrations of 200 μg g−1 as internal standard. The homogeneity of elemental distributions in sample layers deposited on the TXRF quartz carriers by evaporating 5 μL of the 10 mg mL−1 slurries was studied by scanning the 4- to 5-mm-diameter spots of two samples by synchrotron radiation TXRF at Hasylab. For powders with differing graininess but mainly finer than about a few 10 μm, no systematic influence of the grain size on the accuracy of the determinations of Ca, V, Fe, Ni, Cu and Zn could be observed. The measurement precision, however, seemed to be limited by inhomogeneous distributions of the trace elements in the samples as testified by the synchrotron radiation TXRF scans. Detection limits of the developed TXRF procedure for Ca, V, Cr, Mn, Fe, Ni, Cu, Zn and Ga were found to be in the 0.3–7 μg g−1 range and were shown to increase slightly with the grain size of the samples. Quantification using Al (matrix) as internal standard led to systematically higher values out of the accuracy required, whereas the other two approaches in all cases led to reliable results.
Microdrop Deposition Technique: Preparation and Characterization of Diluted Suspended Particulate Samples
The analysis of particulate matter (PM) in dilute solutions is an important target for environmental, geochemical, and biochemical research. Here, we show how microdrop technology may allow the control, through the evaporation of small droplets, of the deposition of insoluble materials dispersed in a solution on a well-defined area with a specific spatial pattern. Using this technology, the superficial density of the deposited solute can be accurately controlled. In particular, it becomes possible to deposit an extremely reduced amount of insoluble material, in the order of few μg on a confined area, thus allowing a relatively high superficial density to be reached within a limited time. In this work, we quantitatively compare the microdrop technique for the preparation of particulate matter samples with the classical filtering technique. After having been optimized, the microdrop technique allows obtaining a more homogeneous deposition and may limit the sample amount up to a factor 25. This method is potentially suitable for many novel applications in different scientific fields such as demanding spectroscopic studies looking at the mineral fraction contained in ice cores or to pollution investigations looking at the detection of heavy metals present in ultra-trace in water.
Neutron Residual Stress Measurements on Rail Sections for Different Production Conditions
Rail sectioning with subsequent neutron diffraction experiments has been used to assess residual stresses in the rails. In this study we present the results of neutron stress measurements performed at the NIST Center for Neutron Research (NCNR) on rail sections from rails that were produced under various conditions. Specifically, these are air-cooled, air-cooled and roller-straightened, head-hardened and head-hardened and roller-straightened. More significantly, a head-hardened and roller-straightened rail was also studied after service to elucidate evolution of the service-induced residual stresses. In the latter case both a transverse-cut slice and the central region of a 0.53 m long piece were studied. Measurements on this piece are the first in which triaxial stresses have been determined for an intact rail. Neutron strain measurements with 3×3×3 mm3 spatial resolution were successfully employed for transversally cut slices to verify the difference in the stress state depending on the production process. Although examination of slices allows determination of only two-dimensional stresses in the plane of the slice, additional measurements on obliquely-cut slices, which were also carried out, and utilization of FEM gives the possibility of reconstructing the full triaxial stress distribution. Together, these approaches provide a better understanding of rail fabrication and the possibility of improving the durability and safety of rails in the future.Copyright © 2004 by ASME