August 2014 Archives

Professor L. Vincze (Ghent University, Belgium) and his colleagues have reported on the latest fluorescence mode XANES imaging using the SLcam, which is an energy dispersive pnCCD detector. At BM26A, ESRF, the measurements were done for iron foil with some oxides and geological standard samples. The typical detection limit and measuring time were 0.5 wt% and 15 h, respectively. Readers might think that energy-resolution can be sacrificed near the absorption edges of interest in order to shorten the measuring time in the same way as ordinary XANES measurement by means of X-ray fluorescence. Although the use of ordinary X-ray CCD in accumulation mode for a very similar experiment was published 10 years ago (for example, M. Mizusawa et al, J. Synchrotron Rad. 11, 209 (2004)), the present system has the advantage of being able to reduce the background from the major light elements contained in the sample. For more information, see the paper, "Full-Field Fluorescence Mode Micro-XANES Imaging Using a Unique Energy Dispersive CCD Detector", P. Tack et al, Anal. Chem., 86, 8791(2014).

Most X-ray experiments can be done at high quality with ease in an ordinary laboratory. Some experiments, however, have to be done in the field. It is hard to imagine a more extreme definition of "in the field" than the planet of Mars, which is why exciting times have come about since NASA's Mars rover "Curiosity" landed on Mars in August 2012. It has since recorded and sent back a large number of datasets including X-ray fluorescence (XRF) and X-ray diffraction (XRD) data. Naturally, the scientists involved with the projects have been speaking globally since. During EXRS 2014 (June, Bologna, Italy), Professor J. L. Campbell (University of Guelph, Canada) gave a keynote lecture entitled "XRF and PIXE on the Mars Science LAB Curiosity Rover". At the Denver X-ray conference (July, Big Sky, Montana), the Plenary Session was "X-rays on Mars", and 3 scientists gave lectures. Professor D. L. Bish (Indiana University) gave a talk entitled "The First X-ray Diffraction Results From Mars". Professor J. L. Campbell's talk on "XRF Combines with PIXE in Curiosity's Alpha Particle X-ray Spectrometer" was the extension on his talk at EXRS 2014, and further detailed and specific discussion was done there. Professor S.M. Clegg talked about "Exploring Mars with ChemCam on the Curiosity Rover" (ChemCam enables quick element determination by the laser-induced plasma emission spectroscopy). In August, at Montreal, during the International Union of Crystallography's congress, Professor D. L. Bish gave a talk entitled "The First X-ray Powder Diffraction Measurements on Mars". These talks highlighted many interesting technological aspects of the measurements: XRF analysis is done first by the same CCD camera, which works as an energy-dispersive 2D X-ray detector, even when the main aim of the measurement is obtaining the XRD pattern. In the analysis of unknown samples, generally both chemical composition and the crystal structure are indispensable. Another reason is that XRF helps the systematic use of single photon counting mode of the CCD camera to get a good quality XRD pattern. Secondly, the samples are vibrated all the time to ensure a smooth and continuous Debye ring. The rover furthermore contains a series of standard samples to check the reliability and reproducibility of the measurements. The readers might be interested in such a compact X-ray analyzer, which combined both XRD and XRF machine. Very similar system is now commercially available. For further information on the scientific activity on Mars, visit the Web page, http://mars.jpl.nasa.gov/msl/

Professor J. Wang (University of California San Diego, USA) and his colleagues have applied X-ray fluorescence to the analysis of gunshot residue, which has been usually detected based on the analysis trace amounts of metallic and organic species deposited on the hands, face, hair, and clothing of the shooter. The researchers tried to couple square-wave stripping voltammetry (SWSV) and scanning electron microscopy (SEM) plus energy dispersive X-ray spectroscopy (EDX). The former method can be used as a rapid screening tool, while the latter contributes to confirmation of the presence of the characteristic morphology and metal composition of gunshot residue particles. For more information, see the paper, "Orthogonal Identification of Gunshot Residue with Complementary Detection Principles of Voltammetry, Scanning Electron Microscopy, and Energy-Dispersive X-ray Spectroscopy: Sample, Screen, and Confirm", A. M. O'Mahony et al., Anal. Chem., 86, 8031 (2014).

A research team led by Professor I. Nakai (Tokyo University of Science, Japan) has recently clarified the detailed chemical nature of radioactive aerosol microparticles emitted during the Fukushima Daiichi Nuclear Power Plant accident. They collected three fine particles of 2 microns in dia, containing radioactive cesium, on March 14th and 15th, 2011, in Tsukuba, 172 km away from the power plant. In addition to Fe, Zn, Rb, Zr, Mo, Sn, Sb, Te, Cs, and Ba, U was detected in two particles. The oxidation states of the heavy elements were also studied by X-ray absorption spectra. The experiments were done at BL37XU, SPring-8, Japan. For more information, see the paper, "Detection of Uranium and Chemical State Analysis of Individual Radioactive Microparticles Emitted from the Fukushima Nuclear Accident Using Multiple Synchrotron Radiation X-ray Analyses", Y. Abe et al., Anal. Chem., 86, 8521 (2014).