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Title: A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

Abstract

The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation,more » the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.« less

Authors:
; ; ;  [1];  [2]
  1. Atominstitut, TU Wien, Stadionallee 2, 1020 Vienna (Austria)
  2. Fuel Chemistry Division, Bhabha Atomic Research Centre (BARC), Mumbai 400085 (India)
Publication Date:
OSTI Identifier:
22482724
Resource Type:
Journal Article
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 86; Journal Issue: 8; Other Information: (c) 2015 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0034-6748
Country of Publication:
United States
Language:
English
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; CARBON; DESIGN; EXCITATION; FLUORESCENCE; SAMPLE CHANGERS; SENSITIVITY; SPECTROMETERS; URANIUM; X RADIATION; X-RAY FLUORESCENCE ANALYSIS; X-RAY SOURCES; X-RAY TUBES

Citation Formats

Wobrauschek, P., E-mail: wobi@ati.ac.at, Prost, J., Ingerle, D., Kregsamer, P., Streli, C., and Misra, N. L. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence. United States: N. p., 2015. Web. doi:10.1063/1.4928499.
Wobrauschek, P., E-mail: wobi@ati.ac.at, Prost, J., Ingerle, D., Kregsamer, P., Streli, C., & Misra, N. L. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence. United States. https://doi.org/10.1063/1.4928499
Wobrauschek, P., E-mail: wobi@ati.ac.at, Prost, J., Ingerle, D., Kregsamer, P., Streli, C., and Misra, N. L. 2015. "A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence". United States. https://doi.org/10.1063/1.4928499.
@article{osti_22482724,
title = {A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence},
author = {Wobrauschek, P., E-mail: wobi@ati.ac.at and Prost, J. and Ingerle, D. and Kregsamer, P. and Streli, C. and Misra, N. L.},
abstractNote = {The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.},
doi = {10.1063/1.4928499},
url = {https://www.osti.gov/biblio/22482724}, journal = {Review of Scientific Instruments},
issn = {0034-6748},
number = 8,
volume = 86,
place = {United States},
year = {Sat Aug 15 00:00:00 EDT 2015},
month = {Sat Aug 15 00:00:00 EDT 2015}
}