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Title: Spatially Resolved Elemental Analysis, Spectroscopy and Diffraction at the GSECARS Sector at the Advanced Photon Source

Abstract

X-ray microprobes (XRM) coupled with high-brightness synchrotron X-ray facilities are powerful tools for environmental biogeochemistry research. One such instrument, the XRM at the Geo Soil Enviro Center for Advanced Radiation Sources Sector 13 at the Advanced Photon Source (APS; Argonne National Laboratory, Lemont, IL) was recently improved as part of a canted undulator geometry upgrade of the insertion device port, effectively doubling the available undulator beam time and extending the operating energy of the branch supporting the XRM down to the sulfur K edge (2.3 keV). Capabilities include rapid, high-resolution, elemental imaging including fluorescence microtomography, microscale X-ray absorption fine structure spectroscopy including sulfur K edge capability, and microscale X-ray diffraction. These capabilities are advantageous for (i) two-dimensional elemental mapping of relatively large samples at high resolution, with the dwell times typically limited only by the count times needed to obtain usable counting statistics for low concentration elements, (ii) three-dimensional imaging of internal elemental distributions in fragile hydrated specimens, such as biological tissues, avoiding the need for physical slicing, (iii) spatially resolved speciation determinations of contaminants in environmental materials, and (iv) identification of contaminant host phases. In this paper, we describe the XRM instrumentation, techniques, applications demonstrating these capabilities, and prospectsmore » for further improvements associated with the proposed upgrade of the APS.« less

Authors:
; ; ; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); National Science Foundation (NSF)
OSTI Identifier:
1346211
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Environmental Quality; Journal Volume: 0; Journal Issue: 0
Country of Publication:
United States
Language:
ENGLISH
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY

Citation Formats

Sutton, Stephen R., Lanzirotti, Antonio, Newville, Matthew, Rivers, Mark L., Eng, Peter, and Lefticariu, Liliana. Spatially Resolved Elemental Analysis, Spectroscopy and Diffraction at the GSECARS Sector at the Advanced Photon Source. United States: N. p., 2017. Web. doi:10.2134/jeq2016.10.0401.
Sutton, Stephen R., Lanzirotti, Antonio, Newville, Matthew, Rivers, Mark L., Eng, Peter, & Lefticariu, Liliana. Spatially Resolved Elemental Analysis, Spectroscopy and Diffraction at the GSECARS Sector at the Advanced Photon Source. United States. doi:10.2134/jeq2016.10.0401.
Sutton, Stephen R., Lanzirotti, Antonio, Newville, Matthew, Rivers, Mark L., Eng, Peter, and Lefticariu, Liliana. Sun . "Spatially Resolved Elemental Analysis, Spectroscopy and Diffraction at the GSECARS Sector at the Advanced Photon Source". United States. doi:10.2134/jeq2016.10.0401.
@article{osti_1346211,
title = {Spatially Resolved Elemental Analysis, Spectroscopy and Diffraction at the GSECARS Sector at the Advanced Photon Source},
author = {Sutton, Stephen R. and Lanzirotti, Antonio and Newville, Matthew and Rivers, Mark L. and Eng, Peter and Lefticariu, Liliana},
abstractNote = {X-ray microprobes (XRM) coupled with high-brightness synchrotron X-ray facilities are powerful tools for environmental biogeochemistry research. One such instrument, the XRM at the Geo Soil Enviro Center for Advanced Radiation Sources Sector 13 at the Advanced Photon Source (APS; Argonne National Laboratory, Lemont, IL) was recently improved as part of a canted undulator geometry upgrade of the insertion device port, effectively doubling the available undulator beam time and extending the operating energy of the branch supporting the XRM down to the sulfur K edge (2.3 keV). Capabilities include rapid, high-resolution, elemental imaging including fluorescence microtomography, microscale X-ray absorption fine structure spectroscopy including sulfur K edge capability, and microscale X-ray diffraction. These capabilities are advantageous for (i) two-dimensional elemental mapping of relatively large samples at high resolution, with the dwell times typically limited only by the count times needed to obtain usable counting statistics for low concentration elements, (ii) three-dimensional imaging of internal elemental distributions in fragile hydrated specimens, such as biological tissues, avoiding the need for physical slicing, (iii) spatially resolved speciation determinations of contaminants in environmental materials, and (iv) identification of contaminant host phases. In this paper, we describe the XRM instrumentation, techniques, applications demonstrating these capabilities, and prospects for further improvements associated with the proposed upgrade of the APS.},
doi = {10.2134/jeq2016.10.0401},
journal = {Journal of Environmental Quality},
number = 0,
volume = 0,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 2017},
month = {Sun Jan 01 00:00:00 EST 2017}
}
  • We have designed and constructed a new system for loading gases at high pressure into diamond anvil cells at pressures up to 200 MPa. The gases are used either as quasi-hydrostatic pressure media surrounding the sample or as the sample itself. The diamond cell is sealed using a clamping mechanism, which permits nearly any type of diamond anvil cell to be used. Online ruby fluorescence and video imaging systems allow in situ monitoring of the pressure and gasket deformation as the cell is sealed, resulting in a very high success rate in loading cells. The system includes interlocks and computermore » control that allow it to be safely and easily operated by visiting users at the Advanced Photon Source. We present preliminary X-ray diffraction data on volume compression of single-crystal magnesium oxide (MgO) in helium up to 110 GPa.« less
  • GSECARS (GeoSoilEnviroCARS, the University of Chicago) operates a bending magnet and an undulator beamlines at Sector 13, Advanced Photon Source. Experimental technique for High Pressure X-ray Tomographic Microscope (HPXTM) using monochromatized X-rays has been developed. The module for HPXTM also has shear deformation capability, which enables us to perform HPXTM experiments for microstructure developed by shear deformation under high pressure. A combination of Deformation DIA (D-DIA) and monochromatic X-rays has been developed for quantitative deformation experiments under pressure above 10 GPa. Deformation experiments of e-iron was performed at pressures up to 19 GPa and temperatures up to 700 K.
  • A photon/safety shutter capable of stopping bremsstrahlung, white, pink, and monochromatic radiation from the APS wiggler and undulator sources is described. The shutter consists of two individually actuated but redundant block assemblies. Each block consists of a water-cooled, OFHC block thermal absorber followed by a tungsten block to stop both synchrotron and bremsstrahlung rays. The design presented here is inexpensive and spatially compact. Fatigue analysis and ANSYS thermal and stress analysis are presented. {copyright} {ital 1996 American Institute of Physics.}
  • The monochromator and focusing mirrors of the 16-BM-D beamline, which is dedicated to high-pressure research with micro-X-ray diffraction (micro-XRD) and X-ray absorption near edge structure (XANES) (6-45 keV) spectroscopy, have been recently upgraded. Monochromatic X-rays are selected by a Si (111) double-crystal monochromator operated in an artificial channel-cut mode and focused to 5 μm × 5 μm (FWHM) by table-top Kirkpatrick-Baez type mirrors located near the sample stage. The typical X-ray flux is ∼5 × 10{sup 8} photons/s at 30 keV. The instrumental resolution, Δq/q{sub max}, reaches to 2 × 10{sup −3} and is tunable through adjustments of the detectormore » distance and X-ray energy. The setup is stable and reproducible, which allows versatile application to various types of experiments including resistive heating and cryogenic cooling as well as ambient temperature compression. Transmission XANES is readily combined with micro-XRD utilizing the fixed-exit feature of the monochromator, which allows combined XRD-XANES measurements at a given sample condition.« less