Centre Européen
de Recherche et d'Enseignement
des Géosciences de l'Environnement

Zoom on ... Synchrotron-based techniques

Explore the matter up to the atomic scale 

Synchrotrons are large instruments that offer extremely bright light, synchrotron radiation, to explore matter and understand its structure and properties. Emitted by electrons circulating at almost the speed of light, this radiation makes it possible to analyze any type of sample down to the scale of the atom.

Many analytical techniques are available in synchrotron. Each year we carry out between 5 and 10 experimental sessions on different beamlines of the ESRF (Grenoble, France), SOLEIL (Paris, France), Elettra (Triestre, Italie), SSRL (Stanford, USA) and APS (Chicago, USA) synchrotrons.

X-ray absorption spectroscopy

XAS (XANES and EXAFS)

X-ray absorption spectroscopy (XAS) is a technique used to determine the speciation of a target element (the absorber atom) present in a solid, liquid or gaseous sample. It is an atomic scale chemical probe, specific to an element. 

XAS is the measurement of transitions from core electronic states of the metal to the excited electronic states and the continuum; the former is known as X-ray absorption near-edge structure (XANES), and the latter as extended X-ray absorption fine structure (EXAFS) which studies the fine structure in the absorption at energies greater than the threshold for electron release. These two methods give complementary structural information, the XANES spectra reporting electronic structure and symmetry of the element site, and the EXAFS reporting numbers, types, and distances to ligands and neighboring atoms from the absorbing element (Koningsberger and Prins 1988).

The beamlines dedicated to the XAS offer various performances and specificities. Some beamlines allow the rapid analysis of concentrated samples with transmission detection mode (eg. XAFS beamline at Elettra). Other beamlines are dedicated to the analysis of highly diluted environmental samples with fluorescence detection mode and multi-element detectors (eg. BM30B-FAME at ESRFSAMBA at SOLEIL or Experimental Station 11-2 at SSRL). Analysis with high energy resolution (HERFD-XAS, eg. BM16-FAME-UHD at ESRF) further increases the sensitivity of the technique. Spatially resolved analyses (micro-XAS) can be performed on beamlines with a micro-focused beam (eg. ID21 at ESRF or LUCIA at SOLEIL).  

X-ray Total scattering with Pair Distribution Function (PDF) Analysis

PDF

Total scattering measurement and analysis by the pair distribution function (PDF) can be used to characterize the local order of amorphous or crystallized systems at short distances.

The radial atomic pair distribution function is calculated by a Fourier transformation of the measured X-ray diffractogram. The pair distribution function describes the probability of finding two atoms separated by a certain distance in the material analyzed. Structural model are then used and tuned to fit the experimental PDF function.

This technique was used in Maureen Le Bars' thesis project (project ANR DIGESTATE) to characterize ZnS nanoparticles that are formed in organic waste. The data were recorded at the APS in Chicago on the beamline ID11-B

More infos ...

... on the techniques in the scientific publications below

High-Energy Resolution Fluorescence Detected X-Ray Absorption Spectroscopy: A Powerful New Structural Tool in Environmental Biogeochemistry Sciences

Journal of Environmental Quality, 2017, DOI:10.2134/jeq2017.01.0023

Auteurs: Proux Olivier Lahera Eric, Net William, Kieffer Isabelle, Rovezzi Mauro, Testemale Denis, Irar Mohammed, Thomas Sara, Aguilar-Tapia Antonio, Bazarkina Elena, Prat Alain, Tella Marie, Auffan Mélanie, Rose Jerome, Hazemann Jean-Louis

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High energy resolution five-crystal spectrometer for high quality fluorescence and absorption measurements on an X-ray Absorption Spectroscopy beamline

Review of Scientific Instruments, 2012, https://doi.org/10.1063/1.4728414

Auteurs: Llorens Isabelle, Lahera Eric, Delnet William, Proux Olivier, Braillard Aurélien, Hazemann Jean-Louis, Prat Alain, Testemale Denis, Dermigny Quentin, Gélébart Frédéric, Morand Marc, Shukla Abhay, Bardou Nathalie, Ulrich Olivier, Arnaud Stephan, Berar Jean-François, Boudet Nathalie, Caillot Bernard, Chaurand Perrine, Rose Jérome, Doelsch Emmanuel, Martin Philippe, Solari Pier Lorenzo

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New methodological approach for the vanadium K-edge X-ray absorption near-edge structure interpretation: Application to the speciation of vanadium in oxide phases from steel slag

Journal of Physical Chemistry B, 2007, DOI: 10.1021/jp063186i

Auteurs: Chaurand Perrine, Rose Jérôme, Briois Valérie, Salomé Murielle, Proux Olivier, Nassif Vivian, Olivi Luca, Susini Jean, Hazemann Jean-Louis, Bottero Jean-Yves

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Some examples of application

Evidence of sulfur-bound reduced copper in bamboo exposed to high silicon and copper concentrations

Environmental Pollution, 2014, DOI: 10.1016/j.envpol.2013.12.02

Auteurs: Collin Blanche, Doelsch Emmanuel, Keller Catherine, Cazevieille Patrick, Tella Marie, Chaurand Perrine, Panfili Frédéric, Hazemann Jean-Louis, Meunier Jean-Dominique

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Investigation of Copper Speciation in Pig Slurry by a Multitechnique Approach

Environmental Science and Technology, 2010, DOI 〈10.1021/es101651w〉

Auteurs: Legros Samuel, Chaurand Perrine, Rose Jerome, Masion Armand, Briois Valérie, Ferrasse Jean-Henry, Saint Macary Hervé, Bottero Jean-Yves, Doelsch Emmanuel

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Chronic dosing of a simulated pond ecosystem in indoor aquatic mesocosms: fate and transport of CeO 2 nanoparticles

Environmental science‎.Nano, 2015, DOI10.1039/c5en00092k〉

Auteurs: Tella M., Auffan M., Brousset L., Morel E., Proux O., Chaneac C., Angeletti B., Paillès C., Artells E., Santaella C., Rose J., Thiéry A., Bottero J.Y.

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Towards a definition of inorganic nanoparticles from an environmental, health and safety perspective

Nature Nanotechnology, 2009, DOI 10.1038/NNANO.2009.242

Auteurs: Auffan M., Rose J., Bottero J.Y., Lowry G., Jolivet J-P., Wiesner M.

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Composition and molecular scale structure of nanophases formed by precipitation of biotite weathering products

Geochimica et Cosmochimica Acta, 2018, https://doi.org/10.1016/j.gca.2018.03.012

Auteurs: Wuhib Zewde Tamrat, Jérôme Rose, Olivier Grauby, Emmanuel Doelsch, Clément Levard, Perrine Chaurand, Isabelle Basile-Doelsch

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