Award Abstract # 1128753
Development of a Tender-Energy Microspectroscopy and Imaging User Facility for Earth Sciences at NSLS and NSLS-II

NSF Org: EAR
Division Of Earth Sciences
Recipient: MIAMI UNIVERSITY
Initial Amendment Date: March 27, 2013
Latest Amendment Date: March 27, 2013
Award Number: 1128753
Award Instrument: Standard Grant
Program Manager: David Lambert
EAR
 Division Of Earth Sciences
GEO
 Directorate for Geosciences
Start Date: April 1, 2013
End Date: March 31, 2015 (Estimated)
Total Intended Award Amount: $1,000.00
Total Awarded Amount to Date: $1,000.00
Funds Obligated to Date: FY 2013 = $1,000.00
History of Investigator:
  • John Rakovan (Principal Investigator)
    rakovajf@miamioh.edu
Recipient Sponsored Research Office: Miami University
501 E HIGH ST
OXFORD
OH  US  45056-1846
(513)529-3600
Sponsor Congressional District: 08
Primary Place of Performance: Miami University
OH  US  45056-2473
Primary Place of Performance
Congressional District:
08
Unique Entity Identifier (UEI): T6J6AF3AM8M8
Parent UEI:
NSF Program(s): Instrumentation & Facilities
Primary Program Source: 01001314DB NSF RESEARCH & RELATED ACTIVIT
Program Reference Code(s):
Program Element Code(s): 158000
Award Agency Code: 4900
Fund Agency Code: 4900
Assistance Listing Number(s): 47.050

ABSTRACT

This project will create a new, unique synchrotron-based user facility to examine geologic materials at the micron scale with a focused X-ray beam tuned specifically for lighter elements Na through Ti. This facility is designed and optimized for "tender" (1-8 keV energy) X-ray micro-spectroscopy and imaging applications for Earth Science research, and will complement existing and highly productive "hard" X-ray facilities operating above about 4.5 keV. It will extend to lower energies the X-ray fluorescence (XRF) and X-ray absorption spectroscopy (XAS) capabilities typical of hard X-ray microprobes, as element-specific non-invasive probes of elemental distribution and local physical and electronic structures and states in crystalline and non-crystalline materials. In addition, it will offer advanced capabilities for microbeam extended X-ray absorption spectroscopy (EXAFS) for determination of more detailed local structure around the selected element.

This project will be undertaken by adding new micro-focusing capabilities at an established and proven macro-focused (~1mm spot size) tender-energy XAS beamline at X15B of the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory, and will subsequently transition to the new Tender Energy Spectroscopy (TES) beamline under development at NSLS-II. Its key attributes will be the distinct 1 to 8 keV energy range, user-tunable spot size from about 50 microns to 1 micron, high flux and stability optimized for high-quality and extended XAS, options for both XRF and XAS mapping with rapid scanning, and a helium glove-box sample environment. Performance will improve when transferred to NSLS-II, a state-of-the-art new Synchrotron designed for high brightness applications. These new capabilities are critical for advancing our knowledge of geochemical and biogeochemical processes, in particular those involving lighter elements, and will be openly available for use through the NSLS General User program. Specific applications targeted include the mineral-water interface, nutrients and contaminants, carbonates, paleoclimate, redox processes, high-pressure mineralogy; and health effects of Earth materials.

PROJECT OUTCOMES REPORT

Disclaimer

This Project Outcomes Report for the General Public is displayed verbatim as submitted by the Principal Investigator (PI) for this award. Any opinions, findings, and conclusions or recommendations expressed in this Report are those of the PI and do not necessarily reflect the views of the National Science Foundation; NSF has not approved or endorsed its content.

This sub-award ($1000) was made to the PI as one of the co-PIs of the larger award for the development of capabilities for tender X-ray spectroscopy on light elements at the NSLS II. The funds were to be used for initial travel to the NSLS.

This report covers only the specific research project that was proposed by the co-PI Rakovan for initial trail experiments in the development of the X15 beamline at the NSLS for subsequent relocation at the NSLS II.

The major activities were Ca and P K-edge EXAFS measurements on hydroxylapatite (HAP), fluorapatite (FAP) and a suite of synthetic amorphous calcium phosphate (ACP) at X15 of the NSLS.

This was done for Ca and P EXAFS characterization of the structurally well constrained model compounds HAP and FAP for comparison to the structurally undetermined ACP for investigation of the existence and structure of nanoclusters in ACP.

The project outcome was the collection of Ca EXAFS. However, because our experiments were scheduled very close to the final shutdown of the NSLS (Mid-September 2014) we encountered serious beam stability problems which rendered quality P EXAFS collection impossible. Ca EXAFS data were collected, but also suggest problems associated with storage ring instability.

Similar measurements were subsequently made at the Siam Photon Source (SPS) in Korak Thailand. The SPS data are quite good and comparison shows that the NSLS data are not usable for structure elucidation. This was a result of facility decomissioning and we do not expect similar propblems at the NSLS II. 

A key outcome is that the experiments supported by this funding are part of the thesis research of M.S. student Aly Hoeher who will be graduation in August from Miami University. 

 


Last Modified: 06/30/2015
Modified by: John F Rakovan

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