Hostname: page-component-76fb5796d-22dnz Total loading time: 0 Render date: 2024-04-26T09:59:36.024Z Has data issue: false hasContentIssue false
  • English
  • Français

EDS Measurements of X-Ray Intensity at WDS Precision and Accuracy Using a Silicon Drift Detector

Published online by Cambridge University Press:  30 July 2012

Nicholas W.M. Ritchie ,
Dale E. Newbury  and
Jeffrey M. Davis
Nicholas W.M. Ritchie*
Affiliation:
Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, MD 20899-8372, USA
Dale E. Newbury
Affiliation:
Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, MD 20899-8372, USA
Jeffrey M. Davis
Affiliation:
Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, MD 20899-8372, USA
*
Corresponding author. E-mail: nicholas.ritchie@nist.gov
Get access

Abstract

The accuracy and precision of X-ray intensity measurements with a silicon drift detector (SDD) are compared with the same measurements performed on a wavelength dispersive spectrometer (WDS) for a variety of elements in a variety of materials. In cases of major (>0.10 mass fraction) and minor (>0.01 mass fraction) elements, the SDD is demonstrated to perform as well or better than the WDS. This is demonstrated both for simple cases in which the spectral peaks do not interfere (SRM-481, SRM-482, and SRM-479a), and for more difficult cases in which the spectral peaks have significant interferences (the Ba L/Ti K lines in a series of Ba/Ti glasses and minerals). We demonstrate that even in the case of significant interference high count SDD spectra are capable of accurately measuring Ti in glasses with Ba:Ti mass fraction ratios from 2.7:1 to 23.8:1. The results suggest that for many measurements wavelength spectrometry can be replaced with an SDD with improved accuracy and precision.

Keywords

EPMAwavelength spectrometrysilicon drift detector (SDD)energy dispersive X-ray spectrometryelectron probe microanalysisWDSZAFquantitative correction
Type
Research Article
Information
Microscopy and Microanalysis , Volume 18 , Issue 4 , August 2012 , pp. 892 - 904
Copyright
Copyright © Microscopy Society of America 2012

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

REFERENCES

Castaing, R. (1951). Application of electron probes to local chemical and crystallographic analysis. PhD Thesis, University of Paris [English translation by P. Duwez and D.B. Wittry, California Institute of Technology, 1955]. Google Scholar
Chantler, C.T., Olsen, K., Dragoset, R.A., Chang, J., Kishore, A.R., Kotochigova, S.A. & Zucker, D.S. (2005). X-ray form factor, attenuation and scattering tables (version 2.1). Available at http://physics.nist.gov/ffast National Institute of Standards and Technology, Gaithersburg, MD. Originally published as Chantler, C.T. (2000). J Phys Chem Ref Data 29(4), 597–1048 and Chantler, C.T. (1995). J Phys Chem Ref Data 24, 71–643. CrossRefGoogle Scholar
Egerton, R.F., Fiori, C.E., Hunt, J.A., Isaacson, M.S., Kirkland, E.J. & Zaluzec, N.J. (1991). EMSA/MAS standard file format for spectral data exchange. EMSA Bulletin 21 35-41. Available at ftp://www.amc.anl.gov/AMC-3/ANLSoftwareLibrary/2-EMMPDL/Xeds/EMMFF/emmff.doc.Google Scholar
Fiorini, C., Kemmer, J., Lechner, P., Kromer, K., Rohde, M. & Schulein, T. (1997). A new detection system for X-ray microanalysis based on a silicon drift detector with Peltier cooling. Rev Sci Instrum 68(6), 2461–2465.CrossRefGoogle Scholar
Gatti, E. & Rehak, P. (1984). Semiconductor drift chamber—An application of a novel charge transport scheme. Nucl Instrum Methods 225, 608.CrossRefGoogle Scholar
Jenkins, R., Manne, R., Robin, R. & Senemaud, C. (1991). Nomenclature, symbols, units and their usage in spectrochemical analysis—VIII. Nomenclature system for X-ray spectroscopy. Pure Appl Chem 63(5), 735–746.CrossRefGoogle Scholar
Kawai, J., Nakajima, K. & Gohshi, Y. (1993). Copper Lβ/Lα X-ray emission intensity ratio of copper compounds and alloys. Spectrochim Acta 48B, 1281–1290.CrossRefGoogle Scholar
Marinenko, R.B., Biancaniello, F., DeRobertis, L., Boyer, P.A. & Ruff, A.W. (1981). Preparation and characterization of an iron-chromium-nickel alloy for microanalysis: SRM 479a. Special Publication 260-70. Washington, DC: National Bureau of Standards. Google Scholar
Meinke, W.W. (1969a). Certificate of analysis, standard reference material 481, gold-silverwires for microprobe analysis. Washington, DC: National Bureau of Standards. Google Scholar
Meinke, W.W. (1969b). Certificate of analysis, standard reference material 482, gold-copper wires for microprobe analysis. Washington, DC: National Bureau of Standards. Google Scholar
Newbury, D., Swyt, C. & Myklebust, R. (1995). Standardless quantitative electron-probe microanalysis with energy dispersive X-ray spectrometry—Is it worth the risk. Analyt Chem 67, 1866–1871.CrossRefGoogle ScholarPubMed
Pouchou, J.L. & Pichoir, F. (1991). Quantitative analysis of homogeneous or stratified microvolumes applying the model “PAP.” In Electron Probe Microanalysis, Heinrich, K.F.J. & Newbury, D.E. (Eds.). New York: Plenum.Google Scholar
Reed, S.J.B. & Ware, N.G. (1973). Quantitative electron microprobe analysis using a lithium drifted silicon detector. X-Ray Spectrom 2, 69–74.CrossRefGoogle Scholar
Ritchie, N.W.M. (2011). Standards-based quantification in DTSA-II—Part 1. Microsc Today 19, 30–36.CrossRefGoogle Scholar
Schamber, F.H. (1977). A modification of the linear least squares fitting method which provides continuum suppression. In X-ray Fluorescence Analysis of Environmental Samples, Dzubay, T. (Ed.). Ann Arbor, MI: Ann Arbor Science.Google Scholar
Statham, P. (1977). Pile-up rejection: Limitations and corrections for residual errors in energy dispersive spectrometers. X-Ray Spectrom 6, 94–103.CrossRefGoogle Scholar