Analytical and Bioanalytical Chemistry

, Volume 407, Issue 11, pp 3045–3053 | Cite as

New reference and test materials for the characterization of energy dispersive X-ray spectrometers at scanning electron microscopes

  • Vanessa Rackwitz
  • Michael Krumrey
  • Christian Laubis
  • Frank Scholze
  • Vasile-Dan HodoroabaEmail author
Research Paper
Part of the following topical collections:
  1. Reference Materials for Chemical Analysis


Checking the performance of energy dispersive X-ray spectrometers as well as validation of the results obtained with energy dispersive X-ray spectrometry (EDX) at a scanning electron microscope (SEM) involve the use of (certified) reference and dedicated test materials. This paper gives an overview on the test materials mostly employed by SEM/EDX users and accredited laboratories as well as on those recommended in international standards. The new BAM reference material EDS-CRM, which is currently in the process of certification, is specifically designed for the characterization of EDS systems at a SEM through calibration of the spectrometer efficiency in analytical laboratories in a simple manner. The certification of the spectra by means of a reference EDS is described. The focus is on the traceability of EDS efficiency which is ensured by measurements of the absolute detection efficiency of silicon drift detectors (SDD) and Si(Li) detectors at the laboratory of the PTB using the electron storage ring BESSY II as a primary X-ray source standard. A new test material in development at BAM for testing the performance of an EDS in the energy range below 1 keV is also briefly presented.


EDX EDS Performance check SEM Test materials Spectrometer efficiency 



Thanks are due to European Metrology Research Programme (EMRP) for funding the SurfChem project (http://www.emrp-surfchem.bam). The EMRP is jointly funded by the EMRP participating countries within EURAMET and the European Union. Many discussions with Dr. M. Procop are gratefully acknowledged by V.-D. H. The authors thank also Dr. W. Bremser (BAM-1.4) for the first evaluation of the homogeneity and stability measurements and Dr. V. Wachtendorf (BAM-7.5) for carrying out the climatic tests.


  1. 1.
    Ritchie NWM, Newbury DE (2012) Uncertainty estimates for electron probe X-ray microanalysis measurements. Anal Chem 84:9956–9962CrossRefGoogle Scholar
  2. 2.
    Scholze F, Procop M (2001) Measurement of detection efficiency and response functions for an Si(Li) x-ray spectrometer in the range 0.1–5 keV. X-Ray Spectrom 30:69–76CrossRefGoogle Scholar
  3. 3.
    Krumrey M, Gerlach M, Scholze F, Ulm G (2006) Calibration and characterization of semiconductor X-ray detectors with synchrotron radiation. Nucl Inst Methods Phys Res A 568:364–368CrossRefGoogle Scholar
  4. 4.
    Statham PJ (1999) Measuring performance of energy-dispersive X-ray systems. Microsc Microanal 4:605–615CrossRefGoogle Scholar
  5. 5.
    Procop M (1996) A simple procedure to check the spectral response of an EDX detector. Mikrochim Acta Suppl 13:473–477Google Scholar
  6. 6.
    Procop M (1999) Estimation of absorbing layer thicknesses for an Si(Li) detector. X-Ray Spectrom 28:33–40CrossRefGoogle Scholar
  7. 7.
    ISO 15632 (2012) Microbeam analysis—selected instrumental performance parameters for the specification and checking of energy-dispersive X-ray spectrometers for use in electron probe microanalysis. ISO, GeneveGoogle Scholar
  8. 8.
    Hodoroaba V-D, Procop M (2014) A method to test the performance of an energy dispersive X-ray spectrometer (EDS). Microsc Microanal 20:1556–1564CrossRefGoogle Scholar
  9. 9.
    ISO/IEC 17025 (2005) General requirements for the competence of testing and calibration laboratories. ISO, GeneveGoogle Scholar
  10. 10.
    BAM Webshop,, Reference Materials/Test Materials
  11. 11.
    Kim KJ, Jang JS, Kim AS, Suh JK, Chung Y-D, Hodoroaba V-D, Wirth T, Unger WES, Kang HJ, Lee YH, Sykes DE, Wang M, Wang H, Ogiwara T, Nishio M, Tanuma S, Simons D, Szakal C, Osborn W, Gorham JM, Steel EB, Terauchi S-y, Kurokawa A, Fujimoto T, Jordaan W, Jeong CS, Havelund R, Spencer S, Shard A, Streeck C, Beckhoff, Eicke A, Terborg R (2014) CCQM-P140 pilot study; Quantitative surface analysis of multi-element alloy films by depth profiling. Metrologia, submittedGoogle Scholar
  12. 12.
    Procop M, Hodoroaba V-D (2009) A test material and a quick procedure for the performance check of X-ray spectrometers attached to the SEM. Microsc Microanal 15(Suppl 2):1120–1121CrossRefGoogle Scholar
  13. 13.
    Hodoroaba V-D, Procop M (2009) Performance check of a wavelength dispersive X-ray spectrometer (WDS) attached to the SEM. Microsc Microanal 15(Suppl 2):1118–1119CrossRefGoogle Scholar
  14. 14.
    Scholze F, Procop M (2009) Modelling the response function of energy dispersive X-ray spectrometers with silicon detectors. X-Ray Spectrom 38:312–321CrossRefGoogle Scholar
  15. 15.
    Kim KJ, Unger WES, Kim JW, Moon DW, Gross T, Hodoroaba V-D, Schmidt D, Wirth T, Jordaan W, Van Staden M, Prins S, Zhang L, Fujimoto T, Song XP, Wang H (2012) Inter-laboratory comparison: quantitative surface analysis of thin Fe-Ni alloy films. Surf Interface Anal 44:192–199CrossRefGoogle Scholar
  16. 16.
    Hodoroaba V-D, Kim KJ, Unger WES (2012) Energy dispersive electron probe microanalysis (ED-EPMA) of elemental composition and thickness of Fe-Ni alloy films. Surf Interface Anal 44:1459–1461CrossRefGoogle Scholar
  17. 17.
    Hodoroaba V-D, Radtke M, Vincze L, Rackwitz V, Reuter D (2010) X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation—modelling experiment, and Monte-Carlo simulation. Nucl Inst Methods Phys Res B 268:3568–3575CrossRefGoogle Scholar
  18. 18.
    Rackwitz V, Panne U, Hodoroaba V-D (2012) Calculation of X-ray tube spectra by means of photon generation yields and a modified Kramers background for side-window X-ray tubes. X-Ray Spectrom 41:264–272CrossRefGoogle Scholar
  19. 19.
    Hodoroaba V-D, Radtke M, Reinholz U, Riesemeier H, Vincze L, Reuter D (2011) X-ray scattering in X-ray fluorescence spectra with X-ray monochromatic, polarised excitation—modelling, experiment, and Monte-Carlo simulation. Nucl Inst Methods Phys Res B 269:1493–1498CrossRefGoogle Scholar
  20. 20.
    Alvisi M, Blome M, Griepentrog M, Hodoroaba V-D, Karduck P, Mostert M, Nacucchi M, Procop M, Rohde M, Scholze F, Statham P, Terborg R, Thiot JF (2006) The determination of the efficiency of energy dispersive X-ray spectrometers by a new reference material. Microsc Microanal 12:406–415CrossRefGoogle Scholar
  21. 21.
    Rackwitz V, Warrikhoff A, Panne U, Hodoroaba V-D (2009) Determination of the efficiency of an energy dispersive X-ray spectrometer up to 50 keV with a SEM. J Anal At Spectrom 24:1034–1036CrossRefGoogle Scholar
  22. 22.
    Burgess S, Li X, Holland J (2013) High spatial resolution energy dispersive X-ray spectrometry in the SEM and the detection of light elements including lithium. Microsc Anal 27(4):S8–S13, EUGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2014

Authors and Affiliations

  • Vanessa Rackwitz
    • 1
  • Michael Krumrey
    • 2
  • Christian Laubis
    • 2
  • Frank Scholze
    • 2
  • Vasile-Dan Hodoroaba
    • 1
    Email author
  1. 1.BAM Federal Institute for Materials Research and TestingBerlinGermany
  2. 2.Physikalisch-Technische Bundesanstalt (PTB)BerlinGermany

Personalised recommendations