Hostname: page-component-cd9895bd7-8ctnn Total loading time: 0 Render date: 2024-12-27T10:10:37.815Z Has data issue: false hasContentIssue false
  • English
  • Français

Measurement of Trace Constituents by Electron-Excited X-Ray Microanalysis with Energy-Dispersive Spectrometry

Published online by Cambridge University Press:  06 May 2016

Dale E. Newbury  and
Nicholas W. M. Ritchie
Dale E. Newbury*
Affiliation:
Materials Measurement Science Division, National Institutes of Standards and Technology, Gaithersburg, MD 20899, USA
Nicholas W. M. Ritchie
Affiliation:
Materials Measurement Science Division, National Institutes of Standards and Technology, Gaithersburg, MD 20899, USA
*
*Corresponding author. dale.newbury@nist.gov
Get access

Abstract

Electron-excited X-ray microanalysis performed with scanning electron microscopy and energy-dispersive spectrometry (EDS) has been used to measure trace elemental constituents of complex multielement materials, where “trace” refers to constituents present at concentrations below 0.01 (mass fraction). High count spectra measured with silicon drift detector EDS were quantified using the standards/matrix correction protocol embedded in the NIST DTSA-II software engine. Robust quantitative analytical results for trace constituents were obtained from concentrations as low as 0.000500 (mass fraction), even in the presence of significant peak interferences from minor (concentration 0.01≤C≤0.1) and major (C>0.1) constituents. Limits of detection as low as 0.000200 were achieved in the absence of peak interference.

Keywords

electron beam X-ray microanalysisenergy-dispersive X-ray spectrometryscanning electron microscopysilicon drift detectortrace analysis
Type
Technique and Instrumentation Development
Information
Microscopy and Microanalysis , Volume 22 , Issue 3 , June 2016 , pp. 520 - 535
Copyright
Copyright © Microscopy Society of America 2016

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Chantler, C.T.J. (2005). Phys. Chem. Ref. Data 2000, 29 (4), 597−1048. Available online as: (b) Chantler, C.T.; Olsen, K.; Dragoset, R.A.; Chang, J.; Kishore, A.R.; Kotochigova, S.A.; Zucker, D.S. X-Ray Form Factor, Attenuation and Scattering Tables, version 2.1 [Online]; National Institute of Standards and Technology: Gaithersburg, MD, 2005. Available at http://physics.nist.gov/ffast.Google Scholar
Currie, L.A. (1968). Limits for qualitative detection and quantitative determination. Anal Chem 40, 586–593.10.1021/ac60259a007Google Scholar
Donovan, J.J., Singer, J.W. & Armstrong, J.T. (2016). A new EPMA method for fast trace element analysis in simple matrices. Am Mineral. (accepted for publication).10.2138/am-2016-5628Google Scholar
Goldstein, J., Newbury, D., Joy, D., Lyman, C., Echlin, P., Lifshin, E., Sawyer, L. & Michael, J. (2003). Scanning Electron Microscopy and X-Ray Microanalysis, 3rd ed.New York: Springer.10.1007/978-1-4615-0215-9Google Scholar
Heinrich, K. (1981). Electron Beam X-Ray Microanalysis. New York: Van Nostrand Reinhold. pp. 99–140.Google Scholar
ISO 22309:2011 (2011). Microbeam Analysis – Quantitative Analysis Using Energy-Dispersive Spectrometry (EDS) for Elements with an Atomic Number of 11 (Na) or Above. Geneva, Switzerland: International Standards Organization. Available at https://www.iso.org/obp/ui/#iso:std:iso:22309:ed-2:v1:en (retrieved 9 March 2016).Google Scholar
National Institute of Standards and Technology (U.S.) Certificate of Analysis, Standard Reference Material 610 (2012). Trace elements in Glass, S.A. Wise and R.L. Watters, Jr. NIST, Gaithersburg, MD, USA.Google Scholar
Newbury, D.E. & Ritchie, N.W.M. (2015 a). Review: Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy dispersive X-ray spectrometry (SEM/SDD-EDS). J. Mater Sci 50, 493–518.10.1007/s10853-014-8685-2Google Scholar
Newbury, D.E. & Ritchie, N.W.M. (2015 b). Quantitative electron-excited x-ray microanalysis of borides, carbides, nitrides, oxides, and fluorides with scanning electron microscopy/silicon drift detector energy-dispersive spectrometry (SEM/SDD-EDS) and NIST DTSA-II. Microsc Microanal 21, 1327–1340.10.1017/S1431927615014993Google Scholar
Pouchou, J.-L. & Pichoir, F. (1995). Quantitative analysis of homogeneous or stratified microvolumes applying the model “PAP”. In Electron Probe Quantitation, K.F.J. Heinrich & D.E. Newbury (Eds.), pp. 31–75. New York: Plenum.Google Scholar
Ritchie, N.W.M. (2015). NIST DTSA-II software, including tutorials. Available at www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html. (retrieved 31 October 2015).Google Scholar
Ritchie, N.W.M. & Newbury, D.E. (2012). Uncertainty estimates for electron probe x-ray microanalysis measurements. Anal Chem 84, 9956–9962.10.1021/ac301843hGoogle Scholar
Ritchie, N.W.M., Newbury, D.E. & Davis, J.M. (2012). EDS measurements at WDS precision and accuracy using a silicon drift detector. Microsc Microanal 18, 892–904.10.1017/S1431927612001109Google Scholar
Rocholl, A., Simon, K., Jochum, K., Bruhn, F., Gehann, R., Kramar, U., Luecke, W., Molzahn, M., Pernicka, E., Seufert, M., Spettel, B. & Stummeier, J. (1997). Chemical characterisation of NIST silicate glass certified reference material SRM 610 by ICP-MS, TIMS, LIMS, SSMS, INAA, AAS, and PIXE. Geostandard Newslett 21, 101–114.10.1111/j.1751-908X.1997.tb00537.xGoogle Scholar
Struder, L., Fiorini, C., Gatti, E., Hartmann, R., Holl, P., Krause, N., Lechner, P., Longoni, A., Lutz, G., Kemmer, J., Meidinger, N., Popp, M., Soltau, H. & van Zanthier, C. (1998). High resolution non dispersive x-ray spectroscopy with state of the art silicon detectors. Mikrochim Acta Suppl 15, 11–19.Google Scholar
Vicenzi, E.P., Eggins, S., Logan, A. & Wysoczanski, R. (2002). Microbeam characterization of corning archeological reference glasses: New additions to the Smithsonian microbeam standard collection. J Res Natl Inst Stand Technol 107, 719–727.10.6028/jres.107.058Google Scholar
Williams, D.B. & Goldstein, J.I. (1981). Artifacts encountered in energy dispersive x-ray spectrometry in the analytical electron microscope. In Energy Dispersive X-Ray Spectrometry, K.F.J. Heinrich, D.E. Newbury, R.L. Myklebust & C.E. Fiori National Bureau of Standards Special Publication 604 (Eds.), pp. 341–349. Washington, DC: U.S. Department of Commerce.Google Scholar