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Quantification of Olivine Using Fe Lα in Electron Probe Microanalysis (EPMA)

Published online by Cambridge University Press:  27 February 2018

Ben Buse*
Affiliation:
School of Earth Sciences, University of Bristol, Bristol BS81RJ, UK
Stuart Kearns
Affiliation:
School of Earth Sciences, University of Bristol, Bristol BS81RJ, UK
*
Author for correspondence: Ben Buse, E-mail: [email protected]
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Abstract

Quantification of first series transition metal Lα X-rays is hampered by absorption and in some cases transition probabilities (fluorescence yields) varying with chemical bonding. Compound mass absorption coefficients for Fe Lα were measured in the olivine solid solution series [Forsterite (Mg2SiO4) to Fayalite (Fe2SiO4)] and the mass absorption coefficients for Fe Lα absorbed by Fe were calculated. The mass absorption coefficients vary systematically between Fo83 and Fo0. Using the measured mass absorption coefficients for both standard and unknown and by correcting for a systematic discrepancy, consistent with varying partial fluorescence yields, a good agreement between calculated k-ratios and measured k-ratios is achieved. The systematic variations allow quantification of unknown k-ratios. The described method of quantification requires modification of matrix correction routines to allow standards and unknowns to have different mass absorption coefficients, and to incorporate solid solution mass absorption coefficients and partial fluorescence yield corrections derived from regression of experimental data.

Type
Materials Science Applications
Copyright
© Microscopy Society of America 2018 

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References

Armstrong, JT (1991) Quantitative elemental analysis of individual microparticles with electron beam instruments. In Electron Probe Quantitation, Heinrich KFJ and Newbury DE (Eds.), pp. 261–315. New York: Plenum Press.Google Scholar
Batanova, V, Sobolev, A, Thompson, J, Danyushevsky, L, Goemann, K, Portnyagin, M, Garbe-Schoenberg, D, Hauri, E, Kimura, J-I, Chang, Q, Senda, R, Chauvel, C, Campillo, S and Ionov, D (2017) Preliminary data on new Olivine reference material MongOL Sh11-2 for in situ microanalysis. Goldschmidt Conference Abstract, Paris, France.Google Scholar
Buse, B and Kearns, SL (2011) Using Fe L X-rays to analyze ferromagnesian minerals. European Microbeam Analysis Society 2011 Conference Abstract, Angers, France.Google Scholar
Buse, B, Kearns, S, Clapham, C and Hawley, D (2016) Decontamination in the electron probe microanalysis with a Peltier-cooled cold finger. Microsc Microanal 22, 981986.Google Scholar
Fialin, M (1990) Some considerations on the use of Lα series of transition metals in electron probe microanalysis: The example of zinc minerals. X-ray Spectrometry 19, 169172.Google Scholar
Fialin, M, Wagner, C, Metrich, N, Humler, E, Galoisy, L and Bezos, A (2001) Fe3+/ΣFe vs. FeLα peak energy for minerals and glasses: Recent advances with the electron microprobe. Am Mineral 86, 456465.Google Scholar
Gopon, P, Fournelle, J, Sobol, PE and Llovet, X (2013) Low-voltage electron probe microanalysis of Fe-Si compounds using soft x-rays. Microsc Microanal 19, 16981708.CrossRefGoogle ScholarPubMed
Hofer, HE and Brey, GP (2007) The iron oxidation state of garnet by electron microprobe: Its determination with the flank method combined with major-element analysis. Am Mineral 92, 873885.Google Scholar
Hovington, P, Drouin, D and Gauvin, R (1997) CASINO: A new Monte Carlo code in C language for electron beam interaction – Part 1: Description of the program. Scanning 19, 119.Google Scholar
Llovet, X, Heikinheimo, E, Nüñez, A, Merlet, C, Almagro, JF, Richter, S, Fournelle, J and van Hoek, CG (2012) An interlaboratory comparison of EPMA analysis of alloy steel at low voltage. IOP Conf Series Mat Sci Eng 32, 012014.Google Scholar
Llovet, X, Pinard, PT, Heikinheimo, E, Louhenkilpi, S and Richter, S (2016) Electron probe microanalysis of Ni silicides using Ni-L X-ray lines. Microsc Microanal 6, 12331243.Google Scholar
Pinard, PT and Richter, S (2016) Quantification of low concentration elements using soft X-rays at high spatial resolution. IOP Conf Ser Mater Sci Eng 109, 012013.Google Scholar
Pouchou, JL and Pichoir, F (1985) Anomalies d’emission et d’absorption du rayonnement Ni La. J Microsc Spectrosc Electron 10, 291294.Google Scholar
Pouchou, JL and Pichoir, FMA (1988) Determination of mass absorption coefficients for soft x-rays by use of the electron microprobe. In Microbeam Analysis, Newbury DE (Ed.), pp. 319324. San Francisco, CA: San Francisco Press.Google Scholar
Remond, G, Myklebust, R, Fialin, M, Nockolds, C, Phillips, M and Roques-Carmes, C (2002) Decomposition of wavelength dispersive X-ray spectra. J Res Natl Inst Stand Technol 6, 509529.CrossRefGoogle Scholar
Statham, P and Holland, J (2014) Prospects for higher spatial resolution quantitative X-ray analysis using transition element L-lines. IOP Conf Ser Mater Sci Eng 55, 012017.Google Scholar
Waldo, RA (1988) An iteration procedure to calculate film compositions and thicknesses in electron-probe microanalysis. In Microbeam Analysis, Newbury DE (Ed.), pp. 310–314. San Francisco, CA: San Francisco Press.Google Scholar