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No Access Submitted: 22 November 2006 Accepted: 14 April 2007 Published Online: 17 May 2007

  • Synchrotron x-ray spectroscopy of Eu∕HNO3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly

Review of Scientific Instruments 78, 053904 (2007); https://doi.org/10.1063/1.2737748
Robert A. Mayanovica)
  • Department of Physics, Astronomy and Materials Science, Missouri State University, Springfield, Missouri 65897
    • Alan J. Anderson
  • Department of Earth Sciences, St. Francis Xavier University, P.O. Box 5000, Antigonish, Nova Scotia B2G 2W5, Canada
    • William A. Bassett
  • Department of Earth and Atmospheric Sciences, Cornell University, Ithaca, New York 14853
    • I-Ming Chou
  • MS 954, U.S. Geological Survey, Reston, Virginia 20192
    • more...View Affiliations

    • a)Author to whom correspondence should be addressed; Fax: (417)-836-6226; electronic mail: [email protected]

    View Contributors
    • Robert A. Mayanovic
    • Alan J. Anderson
    • William A. Bassett
    • I-Ming Chou
    ABSTRACT
    A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to ∼900°C and 700MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam. The supporting rail allows for uniform translation of the HDAC, rotation and tilt stages, and a focusing mirror, which is used to illuminate the sample for visual observation using a microscope, relative to the direction of the incident x-ray beam. A structure study of Eu(III) aqua ion behavior in high-temperature aqueous solutions and a study of Nb partitioning and coordination in a silicate melt in contact with a hydrothermal fluid are described as applications utilizing the modified HDAC rail assembly.

    ACKNOWLEDGMENTS

    The authors wish to thank Steve Heald and Robert Gordon at PNC/XOR beam line and Steve Sutton and Matt Newville at the GeoSoilEnviroCARS beam line, at the Advanced Photon Source (APS). This research was funded by a grant from the NSF EAR-0337338 to one of the authors (R.A.M.) and the Natural Sciences and Engineering Research Council of Canada (NSERC) grant to (A.J.A.) and through a Major Facility Access Grant. The U.S. Department of Energy, Basic Energy Sciences, Office of Science, under Contract Nos. W-31-109-Eng-38 and DE-FG03-97ER45628 (PNC/XOR) supported the use of the APS. GeoSoilEnviroCARS is supported by the National Science Foundation—Earth Sciences (EAR-0217473), Department of Energy—Geosciences (DE-FG02-94ER14466), and the State of Illinois. The authors thank Johnathan Rinck for his assistance with analysis of the Nb silicate melt/H2O system XAS spectra and Robert Seal and Harvey Belkin for their constructive reviews of the manuscript. The use of trade, product, industry, or firm names in this report is for descriptive purpose only and does not constitute endorsement by the U.S. Government.

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