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Application of benchtop micro-XRF to geological materials

Published online by Cambridge University Press:  02 January 2018

Stephanie Flude ,
Michael Haschke  and
Michael Storey
Stephanie Flude*
Affiliation:
Quaternary Dating Laboratory, Environmental and Spatial Change, Roskilde University, Roskilde, Denmark
Michael Haschke
Affiliation:
Bruker AXS, Berlin, Germany (Retired)
Michael Storey
Affiliation:
Quaternary Dating Laboratory, Environmental and Spatial Change, Roskilde University, Roskilde, Denmark
*
*E-mail: sflude@gmail.com
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Abstract

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Recent developments in X-ray optics have allowed the development of a range of commercially available benchtop micro-XRF (μ-XRF) instruments that can produce X-ray spot sizes of 20–30 μm on the sample, allowing major- and trace-element analysis on a range of sample types and sizes with minimal sample preparation. Such instruments offer quantitative analysis using fundamental parameter based 'standardless' quantification algorithms. The accuracy and precision of this quantitative analysis on geological materials, and application of micro-XRF to wider geological problems is assessed using a single benchtop micro-XRF instrument. Quantitative analysis of internal reference materials and international standards shows that such instruments can provide highly reproducible data but that, for many silicate materials, standardless quantification is not accurate.Accuracy can be improved, however, by using a simple type-calibration against a reference material of similar matrix and composition. Qualitative analysis with micro-XRF can simplify and streamline sample characterization and processing for subsequent geochemical and isotopic analysis.

Keywords

micro-XRFgeochemical analysispetrographyelement mappingquantification
Type
Research Article
Information
Mineralogical Magazine , Volume 81 , Issue 4 , August 2017 , pp. 923 - 948
Creative Commons
Creative Common License - CCCreative Common License - BY
© [2017] The Mineralogical Society of Great Britain and Ireland. This is an open access article distributed under the terms of the Creative Commons Attribution (CC BY) licence (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2017

Footnotes

†

Present address: School of Geosciences, The University of Edinburgh, Scotland.

§

Present address: Quadlab, Natural History Museum of Denmark, Copenhagen, Denmark.

References

Bergmann, U., Manning, P.L. and Wogelius, R.A. (2012) Chemical mapping of paleontological and archeo-logical artifacts with synchrotron X-rays. Annual Review of Analytical Chemistry, 5, 361–389.CrossRefGoogle ScholarPubMed
Cauzid, J., Philippot, P., Somogyi, A.,Ménez, B., Simionovici, A. and Bleuet, P. (2006) Standardless quantification of single fluid inclusions using synchrotron radiation induced X-ray fluorescence. Chemical Geology, 227, 165–183.CrossRefGoogle Scholar
Cope, E.D. (1877) A contribution to the knowledge of the ichthyological fauna of the Green River Shales. Bulleting of the United States Geological and Geographical Survey of the Territories, 3, 807–819.Google Scholar
Ebel, H. (1999) X-ray tube spectra. X-Ray Spectrometry, 28, 255–266.3.0.CO;2-Y>CrossRefGoogle Scholar
Elam, W.T., Ravel, B.D. and Sieber, J.R. (2002) A new atomic database for X-ray spectroscopic calcula-tions. Radiation Physics and Chemistry, 63, 121–128.CrossRefGoogle Scholar
Elam, W.T., Shen, R.B., Scruggs, B. and Nicolosi, J. (2004) Accuracy of standardless FP analysis of bulk and thin film samples using a new atomic database. Advances in X-Ray Analysis, 47, 147–109.Google Scholar
Elam, W.T., Shen, R.B., Scruggs, B. and Nicolosi, J. (2006) Full spectrum calculations of EDXRF spectra. Advances in X-Ray Analysis, 49, 261–266.Google Scholar
Fialin, M., Remy, H., Richard, C. and Wagner, C. (1999) Trace element analysis with the electron microprobe: New data and perspectives. American Mineralogist, 84, 70–77.CrossRefGoogle Scholar
Figueiredo, M.O., Ramos, M.T., da Silva, T.P., Basto, M.J. and Chevallier, P. (1999) Synchrotron XRF micro-probe analysis of geological samples: influence of size and orientation of single mineral grains. X-Ray Spectrometry, 28, 251–254.3.0.CO;2-C>CrossRefGoogle Scholar
Flude, S., McGarvie, D.W., Burgess, R. and Tindle, A.G. (2010) Rhyolites at Kerlingarfjöll, Iceland: the evolution and lifespan of silicic central volcanoes. Bulletin of Volcanology, 72, 523–538.CrossRefGoogle Scholar
Flude, S., Lee, M.R., Sherlock, S.C. and Kelley, S.P. (2012) Cryptic microtextures and geological histories of K-rich alkali feldspars revealed by charge contrast imaging. Contributions to Mineralogy and Petrology, 163, 983–994.CrossRefGoogle Scholar
Flude, S., Sherlock, S.C., Lee, M.R. and Kelley, S.P. (2013) Disturbance to the 40Ar/39Ar system in feldspars by electronand ionbeam irradiation. Chemical Geology, 355, 1–12.CrossRefGoogle Scholar
Gorzelak, P., Stolarski, J., Mazur, M. and Meibom, A. (2013) Micro-to nanostructure and geochemistry of extant crinoidal echinoderm skeletons. Geobiology, 11, 29–43.CrossRefGoogle ScholarPubMed
Grande, L. (1982) A revision of the fossil genus Diplomystus with comments on the interrelationships of Clupeomorph fishes. American Museum Novitates, 1–34.Google Scholar
Guilherme, A., Buzanich, G. and Carvalho, M.L. (2012) Focusing systems for the generation of X-ray micro beam: An overview. Spectrochimica Acta Part B: Atomic Spectroscopy, 77, 1–8.CrossRefGoogle Scholar
Haschke, M. and Haller, M. (2003) Examination of poly-capillary lenses for their use in micro-XRF spectrometers. X-Ray Spectrometry, 32, 239–247.CrossRefGoogle Scholar
Hynek, S.A., Brown, F.H. and Fernandez, D.P. (2011) A rapid method for hand picking potassium-rich feldspar from silicic tephra. Quaternary Geochronology, 6, 285–288.CrossRefGoogle Scholar
Ikoma, T., Kobayashi, H., Tanaka, J., Walsh, D. and Mann, S. (2003) Micro structure, mechanical, and biomimetic properties offish scales from Pagrus major. Journal of Structural Biology, 142, 327–333.CrossRefGoogle Scholar
Imayama, T. and Suzuki, K. (2013) Carboniferous inherited grain and age zoning of monazite and xenotime from leucogranites in far-eastern Nepal: Constraints from electron probe microanalysis. American Mineralogist, 98, 1393–1406.CrossRefGoogle Scholar
Jochum, K.P., Stoll, B., Herwig, K., Willbold, M., Hofmann, A.W., Amini, M., Aarburg, S., Abouchami, W., Hellebrand, E., Mocek, B. et al. (2006) MPI-DING reference glasses for in situ microanalysis: New reference values for element concentrations and isotope ratios. Geochemistry Geophysics Geosystems, 7.Google Scholar
Kalsbeek, F., Frei, D. and Affaton, P. (2008) Constraints on provenance, stratigraphic correlation and structural context of the Volta basin, Ghana, from detrital zircon geochronology: An Amazonian connection. Sedimentary Geology, 212, 86–95.CrossRefGoogle Scholar
Kalvoda, J., Novák, M., Bábek, O., Brzobohatý, R., Holá, M., Holoubek, I., Kanický, V and Škoda, R. (2009) Compositional changes in fish scale hydroxylapatite during early diagenesis; an example from an abandoned meander. Biogeochemistry, 94, 197–215.CrossRefGoogle Scholar
Kanngießer, B. (2003) Quantification procedures in micro X-ray fluorescence analysis. Spectrochimica Acta Part B: Atomic Spectroscopy 58, 609–614.CrossRefGoogle Scholar
Kempenaers, L., Janssens, K., Jochum, K.P., Vincze, L., Vekemans, B., Somogyi, A., Drakopoulos, M. and Adams, E (2003) Micro-heterogeneity study of trace elements in USGS, MPI-DING and NIST glass reference materials by means of synchrotron micro-XRF. Journal of Analytical Atomic Spectrometry, 18, 350–357.CrossRefGoogle Scholar
Lanzing, W.J.R. and Wright, R.G. (1976) The ultrastruc-ture and calcification of the scales of Tilapia mossambica (Peters). Cell and Tissue Research, 167, 37–7.CrossRefGoogle Scholar
Lipman, P.W and McIntosh, W.C. (2008) Eruptive and noneruptive calderas, northeastern San Juan Mountains, Colorado: Where did the ignimbrites come from. Geological Society of America Bulletin, 120, 771–795.CrossRefGoogle Scholar
Newbury, D.E. and Ritchie, N.W.M. (2013) Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative. Scanning, 35, 141–168.CrossRefGoogle ScholarPubMed
Newbury, D.E., Swyt, C.R. and Myklebust, R.L. (1995) “Standardless” quantitative electron probe micro-analysis with energy-dispersive X-ray spectrometry: Is it worth the risk. Analytical Chemistry, 67, 1866–1871.CrossRefGoogle Scholar
Padilla, R., Van Espen, P., Abrahantes, A. and Janssens, K. (2005) Semiempirical approach for standardless calibration in (J.-XRF spectrometry using capillary lenses. X-Ray Spectrometry, 34, 19–27.CrossRefGoogle Scholar
Pereira, A.M.T. and Brandao, P.R.G. (2001) Statistical validation of standardless and standard-based analysis by X-ray fluorescence spectrometry in iron ores characterisation. Minerals Engineering, 14, 1659–1670.CrossRefGoogle Scholar
Perrett, G.M., Campbell, J.L., Glasauer, S. and Pardo, R. (2014) Quantitative determination of mineral phase effects observed in APXS analyses of geochemical reference materials: Quantitative determination of mineral phase effects in APXS analyses. X-Ray Spectrometry, 43, 359–366.CrossRefGoogle Scholar
Potts, P.J. and Webb, P.C. (1992) X-ray fluorescence spectrometry. Journal of Geochemical Exploration, 44, 251–296.Google Scholar
Prior, D.J., Trimby, P.W. and Weber, U. (1996) Orientation contrast imaging of microstructures in rocks using forescatter detectors in the scanning electron microscope. Mineralogical Magazine, 60, 859–869.CrossRefGoogle Scholar
Pyle, J.M. (2005) Contributions to precision and accuracy of monazite microprobe ages. American Mineralogist, 90, 547–577.CrossRefGoogle Scholar
Rousseau, R.M. (2006) Corrections for matrix effects in X-ray fluorescence analysis-A tutorial. Spectrochimica Acta PartB: Atomic Spectroscopy, 61, 759–777.CrossRefGoogle Scholar
Rousseau, R.M. (2009) The quest for a fundamental algorithm in X-ray fluorescence analysis and calibration. The Open Spectroscopy Journal, 3, 31–42.CrossRefGoogle Scholar
Schmidt, C., Wirth, R., Wilke, M., Mrosko, M. and Appel, K. (2012) Reactions of strontium anorthite with H2O+CaCl2 fluids at 500 °C and high pressure: Kinetic information from in situ synchrotron-radiation XRF analyses of the fluid. American Mineralogist, 97, 1700–1707.CrossRefGoogle Scholar
Sherman, J. (1955) The theoretical derivation of fluorescent X-ray intensities from mixtures. Spectrochimica Acta, 7, 283–306.CrossRefGoogle Scholar
Smith, M.E., Carroll, A.R. and Singer, B.S. (2008) Synoptic reconstruction of a major ancient lake system: Eocene Green River Formation, western United States. Geological Society of America Bulletin, 120, 54–84.CrossRefGoogle Scholar
Storey, M., Roberts, R.G. and Saidin, M. (2012) Astronomically calibrated 40Ar/39Ar age for the Toba supereruption and global synchronization of late Quaternary records. Proceedings of the National Academy of Sciences. Google Scholar
Whalley, P., Kelley, S.P and Tindle, A.G. (2011) The role of the virtual microscope in distance learning. Open Learning: The Journal of Open, Distance and e-Learning, 26, 127–134.CrossRefGoogle Scholar
Wilson, S.A. (1998a) Data compilations and statistical analysis of intralaboratory results for AGV-2, United States Geological Survey. OpenFileReport(in progress).Google Scholar
Wilson, S.A. (1998b)Datacompilationsfor USGS reference material GSP-2, Granodiorite, Silver Plume Colorado, United States Geological Survey. Open-File Report (in progress).Google Scholar
Wilson, S.A. (2000) Data compilations forUSGS reference material BHVO-2, Hawaiian Basalt, United States Geological Survey. OpenFileReport(in progress).Google Scholar
Wogelius, R.A., Manning, P.L., Barden, H.E., Edwards, N.P., Webb, S.M., Sellers, W.I., Taylor, K.G., Larson, P.L., Dodson, P., You, H. et al. (2011) Trace Metals as Biomarkers for Eumelanin Pigment in the Fossil Record. Science, 333, 1622–1626.CrossRefGoogle ScholarPubMed
Wolff, T., Malzer, W., Mantouvalou, I., Hahn, O. and Kanngießer, B. (2011) A new fundamental parameter based calibration procedure for micro X-ray fluorescence spectrometers. Spectrochimica Acta Part B: Atomic Spectroscopy, 66, 170–178.CrossRefGoogle Scholar
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