Micro analysis of heterogeneous aerosol particles - X-Ray News

So far, high-resolution microscopic analysis of individual atmospheric particles has been fairly difficult because of problems with the filters used for capturing particles.  The research group in the National Institute for Standards and Technologies, United States, is proposing a multiplatform approach for microscopically assessing chemical and optical properties of individual heterogeneous urban dust particles.  The procedures described in the paper could also be useful for similar analysis.  The method uses 5 steps; (i) particles embedded in fibrous filters are transferred to polished silicon/germanium wafers with electrostatically-assisted high-speed centrifugation, (ii) particles with light absorbing/scattering behavior are identified from bright/dark field light-microscopy, (iii) particles identified from light microscopy are compositionally mapped at high-definition with field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy, (iv) compositionally-mapped particles are further analyzed with focused ion-beam (FIB) tomography whereby a series of thin slices from a particle are imaged, and the resulting image stack is used to construct a 3-dimensional model of the particle, and (v) particle chemistry is assessed over two distinct regions of a thin FIB slice of a particle with energy-filtered transmission electron microscopy (TEM) and electron energy-loss spectroscopy associated with scanning TEM.  For more information, see the paper, "Qualitative Multiplatform Microanalysis of Individual Heterogeneous Atmospheric Particles From High-Volume Air Samples", J. M. Conny et al., Anal. Chem., Just Accepted (DOI: 10.1021/ac5022612 Publication Date (Web): September 14).

Full-field XANES imaging - X-Ray News

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).

X-ray analysis on Mars is hot - X-Ray News

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/

Gunshot residue analysis by X-ray fluorescence - X-Ray News

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).

Denver X-ray conference awards - X-Ray News

During the plenary session of the 65th Annual Denver X-Ray Conference, two awards were presented.  The 2014 Birks Award was presented to George Havrilla, Los Alamos National Laboratory for his many contributions to microXRF, especially the development of the confocal XRF microscope. Dr. Havrilla has been a leader in the field of analytical XRF; including 19 years on the Denver X-ray Conference Organizing Committee; nine years as North American Editor of X-ray Spectrometry; and six years as Co-Editor-in-Chief for Advances in X-ray Analysis.  The ICDD Fellow Award was presented to John Getty, Instructor in Geophysical Engineering and Principal Investigator in the Proppant Research Group at Montana Tech. John has played a key role in the planning and execution of the Denver X-ray Conference for more than 30 years.  For further information, visit the Web page, http://www.dxcicdd.com/

It is now known that X-ray free-electron lasers can produce ultrafast X-ray pulses as short as 3 fs in FWHM.  Scientists at the Linac Coherent Light Source (LCLS), Stanford are trying to reduce delay time errors in optical-pump & X-ray probe measurements to the 1 fs level, by 2D spectrogram measurement of the relative X-ray/optical delay.  For more information, see the paper, "Sub-femtosecond precision measurement of relative X-ray arrival time for free-electron lasers", N. Hartmann et al., Nature Photonics, 8, 706 (2014).

Professor T. M. Cahill (Arizona State University) and his colleagues have recently compared the performance of the different excitation modes of synchrotron radiation X-ray fluorescence.  The research team evaluated four different beamline configurations for the analysis of three representative environmental samples; a thin aerosol sample, an intermediate thickness biological sample, and a thick rare earth mineral specimen.  They found that white beam excitation is optimal for the analysis of thin samples with little mass, and that filtered white beam excitation (removing lower energy X-rays by absorber) gives better sensitivity for elements emitting more energetic X-rays.  In their study, monochromatic excitation, which tends to be the standard mode of operation, did not give good results in terms of sensitivity.  For more information, see the paper, "Evaluation of Different Synchrotron Beamline Configurations for X.ray Fluorescence Analysis of Environmental Samples", S. R. Barberie et al., Anal. Chem., 86, 8253 (2014).
A Spanish group has recently published a very interesting application of total-reflection X-ray fluorescence (TXRF).  The research team has evaluated the bioaccumulation kinetics of gold nanorods (GNRs) in various tissues upon intravenous administration in mice.  It was found that the main achievement was clearly differentiating two kinds of behaviors; gold nano rods were quickly bioaccumulated by highly vascular filtration organs such as the liver and spleen, while they do not show bioaccumulation rates in the brain and lung for the period of time investigated.  For more information, see the paper, "Evaluation of Bioaccumulation Kinetics of Gold Nanorods in Vital Mammalian Organs by Means of Total Reflection X-Ray Fluorescence Spectrometry", R. Fernandez-Ruiz et al., Anal. Chem., 86, 7383 (2014).

Dr. V-D. Hodoroaba (BAM, Berlin, Germany) and his colleague have published a report on the feasibility of quantitative X-ray fluorescence (XRF) analysis using coherent (Rayleigh) and incoherent (Compton) X-ray scattering.  They have evaluated the ratio of the Compton-to-Rayleigh intensity observed in XRF spectra and also have discussed its relation to the average atomic number.  In so-called reference-free XRF analysis, which uses only fundamental parameters and a theoretical formula and does not rely on the calibration curve, there still exist many difficulties, particularly for matrices of lower mean atomic numbers.  The analysis presented in this research has sufficiently high sensitivity to distinguish the average atomic number of specimens even within the 0.1 difference.  For more information, see the paper, "Gaining Improved Chemical Composition by Exploitation of Compton-to-Rayleigh Intensity Ratio in XRF Analysis", V-D. Hodoroaba et al., Anal. Chem., 86, 6858 (2014).

YouTube videos of Ultrafast X-ray Summer Seminar 2014 - X-Ray News

he Ultrafast X-ray Summer Seminar (UXSS) 2014 took place from June 15 to 19 at SLAC National Accelerator Laboratory, California, United States.  The program is organized specifically to train students and post-docs on new opportunities in ultrafast science, particularly using X-ray Free Electron Lasers.  Almost all the lectures presented by expert scientists are now available as videos on YouTube.  The lecture by Dr. Pieter Glatzel (ESRF) on "Hard X-ray Spectroscopy" (https://www.youtube.com/watch?v=0sMD8lZzuTE) is surely useful for young X-ray spectroscopists.  Other exciting lectures are available from Dr. Oleg Shpyrko (UCSD) on "Coherent X-ray Scattering at Ultrafast Timescales" (https://www.youtube.com/watch?v=OIR_ltSOl2U), Dr. Michael Odelius (Stockholm University) on "Electronic Structure & Ultrafast Solution Dynamics in Xray vision w/ theoretical spectacles" (https://www.youtube.com/watch?v=ITIzAmYuyWA), Dr. Alexander Fohlisch (Helmholtz Zentrum Berlin) on "Soft X-ray General and Solid State Aspects" (https://www.youtube.com/watch?v=xTz1oCV5cWI), Dr. Philippe Wernet (Helmholtz Zentrum Berlin) on "Ultrafast Molecular Spectroscopy with X-rays: Experiment", and Prof. Claudio Pellegrini (UCLA) on "X-ray Free Electron Lasers" (https://www.youtube.com/watch?v=5v68nuOTwns).  For more information on this summer seminar, visit the following Web site, https://conf-slac.stanford.edu/uxss-2014/
Dr. B. Kanngießer (Technische Universität Berlin, Germany) and her colleagues have recently reported an interesting archaeological application of 3D chemical analysis based on confocal X-ray absorption near edge spectroscopy.  This is highly significant for clarifying the technological background of the decorated black- and red-figured Athenian vases (6th and 5th century BC) and the plain black glaze.  The research team discussed the correlation of the iron oxidation state in the black glaze layer with the manufacturing process.  The 3-stage firing process, which was used in the modern reproduction, was retraced by correlating selected attic black glazed (BG) specimens from different periods (Archaic, Classical, Hellenistic).  For more information, see the paper, "Confocal XANES and the Attic Black Glaze: The Three Stage Firing Process through Modern Reproduction", L. Luhl et al., Anal. Chem., Article ASAP (DOI: 10.1021/ac500990k).

X-ray frequency comb - X-Ray News

So far, laser combs in visible light wavelength have been known as an extremely precise measure of dimensions.  What would happen if they move into the X-ray region?  The advent of an X-ray free electron laser (XFEL) may realize an X-ray frequency comb in the near future.  Dr. S. M. Cavalettobe (Max-Planck-Institut fur Kernphysik, Heidelberg, Germany) is proposing such an ambitious experiment.  The research could open up wide-ranging applications; ultraprecise X-ray atomic clocks, determination of many X-ray fundamental parameters, quantitative understanding of astrophysical models and quantum electrodynamics etc.  For more information, see the paper, "Broadband high-resolution X-ray frequency combs", S. M. Cavaletto et al, Nature Photonics, June 2014 (DOI: 10.1038/nphoton.2014.113).

Synchrotron imaging of birds' ancestor - X-Ray News

At ESRF in Grenoble, France, several very interesting imaging experiments are going on.  Some fossils of Archaeopteryx, which were believed to live 150 million years ago, are being imaged by using a pin-hole X-ray camera at synchrotron beamlines BM5 and ID19.  The main question is about their wings - whether they could fly or not.  So far, the research has encountered a number of challenges.  The project is conducted by Germany's Burgermeister-Muller-Museum (the Solnhofen Museum).  For more information, see the following Web site, http://www.solnhofen.de/index.php?id=0,49

The use of X-ray free-electrons has enabled plenty of fascinating science, such as watching non-equilibrium excited-state dynamics in complexes of 3d transition metals.  Scientists at LCLS, Stanford have performed femtosecond resolution X-ray fluorescence spectroscopy, with its sensitivity to spin state, elucidating the spin crossover dynamics of [Fe(2, 2ˈ-bipyridine)3]2+ on photoinduced metal-to-ligand charge transfer excitation.  For more information, see the paper, "Tracking excited-state charge and spin dynamics in iron coordination complexes", W. Zhang et al., Nature, 509, 345 (2014).

Electrochemical X-ray fluorescence - X-Ray News

A group led by Prof. Julie V. Macpherson (Warwick University, England) has reported electrochemical X-ray fluorescence, which can quantitatively detect heavy metals in solution.  In this technique, electrochemical preconcentration of a species of interest onto the target electrode is achieved by cathodic electro-deposition.  X-ray fluorescence can then help unambiguous elemental identification and quantification of metal concentration.  The key is that the electrochemical preconcentration step improves the detection limit by over 4 orders of magnitude, and it can reach the sub-ppb level.  For more information, see the paper, "Electrochemical X-ray Fluorescence Spectroscopy for Trace Heavy Metal Analysis: Enhancing X-ray Fluorescence Detection Capabilities by Four Orders of Magnitude", L. A. Hutton et al., Anal. Chem., 86, 4566 (2014).

Application of TXRF to the determination of halide in liquid - X-Ray News

Prof. K. Binnemans (KU Leuven, Heverlee, Belgium) and his colleagues have published several papers on the application of TXRF to the determination and quantification of halide impurities in liquid.  So far, the detection of halide ions in solution has been problematic because volatile hydrogen halide compounds are formed when the sample is mixed with the acidic metal standard solution. The loss of hydrogen halide during the drying step of the sample preparation procedure gives imprecise and inaccurate results.  To avoid this, the research group is proposing to introduce an alkaline copper standard Cu(NH3)4(NO3)2.  For more information, see the papers, "Determination of Halide Impurities in Ionic Liquids by Total Reflection X-ray Fluorescence Spectrometry", T. V. Hoogerstraete et al., Anal. Chem., 86, 3931 (2014), and "Determination of Halide Ions in Solution by Total Reflection X-ray Fluorescence (TXRF) Spectrometry", T. V. Hoogerstraete et al., Anal. Chem., 86, 1391 (2014).

Podcast on wavelength-dispersive X-ray fluorescence spectroscopy - X-Ray News

An interesting and useful tutorial on X-ray analytical methods for newcomers is now available in the Materials Today Podcast.  Dr. Ravi Yellepeddi (Thermo Fisher Scientific) explains the principle of X-ray fluorescence, recent progress in instruments, and the variety of applications in industry and research laboratories.  The talk is around 30 min.  Visit the following Web site,


An interesting application of confocal micro-X-ray fluorescence has been reported by Dr. Tianxi Sun (Beijing Normal University, China) and his colleagues.  The technique employs a polycapillary focusing X-ray lens and a polycapillary parallel X-ray lens, as well as the laboratory X-ray source (Mo tube).  In the present research, the scan of the confocal point can give the Cu2+ ion distribution near the surface of the electrode in a steady-state diffusion in an electrolytic tank.  The research group studied the effects of the concentration of the electrolyte and the bath voltage on the shape of the layer on the nonuniform distribution of the Cu2+ ions.  For more information, see the paper, "Spatially Resolved In Situ Measurements of the Ion Distribution Near the Surface of Electrode in a Steady-State Diffusion in an Electrolytic Tank with Confocal Micro X-ray Fluorescence", S. Peng et al., Anal. Chem., 86, 362 (2014).

10th Ewald prize - A. Janner and T. W. J. M. Janssen - X-Ray News

The International Union of Crystallography (IUCr) has announced that Professors A. Janner and T. W. J. M. Janssen (both from the Institute for Theoretical Physics, University of Nijmegen, The Netherlands) have been awarded the tenth Ewald prize for the development of superspace crystallography and its application to the analysis of aperiodic crystals.  The presentation of the Ewald Prize will be made during the Montreal Congress Opening Ceremony on 5 August 2014.  The Ewald prize consists of a medal, a certificate and an award of USD 30,000.  Former recipients are E. Dodson (UK), C. Giacovazzo (Italy), G. M. Sheldric (Germany) in 2011, D. Sayre (USA, 2008), P. Coppens (USA, 2005), M. M. Woolfson (UK, 2002), G. N. Ramachandran (India, 1999), M. G. Rossmann (USA, 1996), N. Kato (Japan, 1993), B. K. Vainshtein (Russia, 1990), J. M. Cowley (USA) and A. F. Moodie (Australia) in 1987.    For further information, visit the Web page, http://www.iucr.org/people/ewald-prize/10th-ewald-prize

The 8th Asada award - X-Ray News

The recipient of the 8th Asada Award, which is presented by the Discussion Group of X-ray Analysis, Japan, in memory of the late Professor Ei-ichi Asada (1924-2005) to promising young scientists in X-ray analysis fields in Japan, is Dr. Hironori Ohashi (Kyushu Univ.), "Characterization of gold catalysts by the combined use of X-ray and Mossbauer spectroscopy"). The ceremony was held during the 49th Annual Conference on X-Ray Chemical Analysis and the 15th International Conference on Total Reflection X-Ray Fluorescence Analysis and Related Methods (TXRF2013), at Osaka City University, Osaka.

Denver X-ray conference awards - X-Ray News

During the plenary session of the 63rd Annual Denver X-Ray Conference, three awards were presented.  The 2013 Barrett Award was presented to Vaclav Petricek of the Institute of Physics, Academy of Sciences of the Czech Republic, Praha, Czech Republic, for developing the theory of incommensurate/modulated/composite crystal structures and its implementation in the computing system Jana2006 (the most widely-used system for solving and refining aperiodic structures), and for making possible the correct archival of such structures in the Powder Diffraction FileTM".  The 2013 Jenkins Award was presented to Rene Van Grieken of the University of Antwerp, Antwerp, Belgium, for contributions to the development and application of X-ray methods to a wide variety of topics, from aerosols in the environment to conservation and from new techniques and microanalysis to biomedical applications.  He has been a leader in the X-ray community and has served it in many capacities over the years, including Editor-in-Chief of X-ray Spectrometry as well as being a member of various national and international commissions involved in analytical and environmental chemistry.  He has disseminated his knowledge in an impressive list of papers, books, and invited lectures.  The 2013 Hanawalt Award was presented to Robert B. Von Dreele of Argonne National Laboratory, Lemont, IL, USA, for his insight, courage and creativity in bringing powder diffraction to the macromolecular community.  For further information, visit the Web page, http://www.dxcicdd.com/

The 2013 Compton award - X-Ray News

The Advanced Photon Source (APS) and APS Users Organization have announced that the 2013 Arthur H. Compton Award has been presented jointly to David E. Moncton, John N. Galayda, Michael Borland, and Louis Emery. The award recognizes the recipients' visionary leadership and technical ingenuity in introducing "top-up" operation to the synchrotron radiation community.  The award consists of a plaque and $2500.  Former recipients of this award are: Edward Stern, Farrel Lytle, Dale Sayers (posthumously), John Rehr (2011); Simon Mochrie, Mark Sutton, Gerhard Grubel  (2009); Andrzej Joachimiak, Gerold Rosenbaum (2007); Gunter Schmahl and Janos Kirz (2005); Martin Blume, Doon Gibbs, Kazumichi Namikawa, Denis McWhan (2003); Wayne A. Hendrickson (2001); Sunil K. Sinha (2000); Donald H. Bilderback, Andreas K. Freund, Gordon S. Knapp, Dennis M. Mills (1998); Philip M. Platzman, Peter M. Eisenberger (1997); Nikolai Vinokurov, Klaus Halbach (1995).

Professor Y. Takahashi (Osaka University, Japan) and his colleagues have recently reported that coherent X-ray imaging using Bragg diffraction can aid the observation of nanoscale dislocation strain fields in a silicon single crystal.  The experiments were done with 11.8 keV micro-focused X-ray photons, around 1 μm in both directions, using KB mirrors at BL-29XUL, SPring-8, Japan.  In this research, a 1 μm thick silicon (100) single crystal was placed in the X-ray path so that X-rays could pass through it and the 220 Bragg reflection spot was observed by a CCD camera 2 m behind the sample. The sample was scanned in XY directions as well.  The research team found phase singularities, i.e., two pairs of vortices with opposite directions in the phase map, that corresponded to the locally dark positions in the intensity map.  It was concluded that this corresponded to the projection of the {111} dislocation loops.  For more information, see the paper, "Bragg x-ray ptychography of a silicon crystal: Visualization of the dislocation strain field and the production of a vortex beam", Y. Takahashi et al., Phys. Rev. B87, 121201(R) (2013).

Final magnet girders installed at NSLS II, Brookhaven - X-Ray News

The construction of Brookhaven's National Synchrotron Light Source II is approaching its final stage. Recently the last of 150 magnet girders was installed in the storage ring.  Magnets traveled from across the globe, supplied by ring magnet vendors based in six countries: Buckley Systems Ltd (New Zealand), Budker Institute of Nuclear Physics (Russia), Danfysik (Denmark), Everson Tesla Incorporated (U.S.), Institute of High Energy Physics (China), and Tesla Engineering (U.K.).  In the experimental hall, meanwhile, 17 hutches have been delivered and constructed for seven beamlines; CSX1 and CSX2 (two branches of Coherent Soft X-ray Scattering and Polarization),     CHX (Coherent Hard X-ray Scattering), IXS (Inelastic X-ray Scattering), HXN (Hard X-ray Nanoprobe), SRX (Submicron Resolution X-ray Spectroscopy) and XPD (X-ray Powder Diffraction).  For further information, visit the Web page, http://www.bnl.gov/ps/news/news.php?a=23725

  An explanation of the CSX beamline construction can be viewed on You Tube.


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