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Characterizing fundamental parameter-based analysis for soil–ceramic matrices in polarized energy-dispersive X-ray fluorescence (PEDXRF) spectrometry

Published online by Cambridge University Press:  07 May 2014

Waleed Amin Abuhani ,
Nabanita Dasgupta-Schubert  and
Luis Manuel Villaseñor Cendejas
Waleed Amin Abuhani*
Affiliation:
Institute of Physics and Mathematics (IFM), University of Michoacan (UMSNH), Morelia, Mexico, Michigan 58060
Nabanita Dasgupta-Schubert
Affiliation:
Institute of Chemical Biology (IIQB), University of Michoacan (UMSNH), Morelia, Mexico, Michigan 58060
Luis Manuel Villaseñor Cendejas
Affiliation:
Institute of Physics and Mathematics (IFM), University of Michoacan (UMSNH), Morelia, Mexico, Michigan 58060
*
a)Author to whom correspondence should be addressed. Electronic mail: abuhani.waleed@gmail.com
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Abstract

Analytical polarized energy-dispersive X-ray fluorescence (PEDXRF) spectrometry (PEDXRFS) represents a substantial advancement over conventional XRF. The higher signal-to-noise commensurate with background lowering and better energy resolution, permits trace analysis for elements with Z ≥ 11. Concomitantly, improvements in analytical software based on the fundamental parameters (FP) approach have improved accuracies and precisions for standard-less analysis (SLA). Two ceramic and soil standard reference materials (SRMs), 98a-Plastic Clay and GSS-1 powders, differed in their intrinsic matrix properties of grain size, bulk, and surface monolayer densities as well as the elemental concentrations. The SRMs were analyzed as powder and as pellets compacted under the same pressure conditions to double the bulk density. Different geometries represented by the sample cup (10, 15, and 24 mm) and pellet (10, 15, and 25 mm) diameters with the same sample thickness (with differing masses and aspect ratios), as well as (for powder samples only) identical low masses (0.5 g) but with varying thicknesses, were analyzed. PEDXRFS combined with TURBOQUANT® (TQ) as SLA-FP enables good quantitative analysis for powders (Z ≥ 13) even for masses significantly lower than recommended, for soil–ceramic samples. Pellets (Z ≥ 12) yielded the best accuracy factor (AF) at high aspect ratio and thicknesses of the matrix analytical depth. Binder in pellets depreciates the AF. TQ needs to adequately quantitate matrix interferences effects, to improve accuracy in the analysis of low atomic numbers, e.g. Na and Mg.

Keywords

XRFfundamental parametersstandard-less analysisstandard reference materials
Type
Technical Articles
Information
Powder Diffraction , Volume 29 , Issue 2 , June 2014 , pp. 159 - 169
Copyright
Copyright © International Centre for Diffraction Data 2014 

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References

Ajay, S. and Rohit, S. (2012). “Validation of analytical procedures: a comparison of ICH vs pharmacopoeia (USP) vs FDA,” Int. Res. J. Pharm. 3(6), 39–42.Google Scholar
Briggs-Kamara, M. A. (2012). “Elemental analysis of selected epidermal creams by x-ray fluorescence (XRF) spectrometry,” Int. J. Emerging Technol. Adv. Eng. 2(5), ISSN 2250-2459.Google Scholar
Brouwer, P. (Ed.) (2010). Theory of XRF: Getting Acquainted with the Principles (PANalytical B.V. Almelo, Netherlands), 3rd ed.Google Scholar
Chan, C. C. (2008). “Analytical method validation: principles and practices,” in Pharmaceutical Manufacturing Handbook: Regulations and Quality, edited by Gad, S. C. (John Wiley & Sons, Inc., Hoboken, NJ, USA), vol. 2, pp. 727–742.Google Scholar
De Francesco, A. M., Crisci, G. M., and Bocci, M. (2008). “Non-destructive analytic method using XRF for determination of provenance of archaeological obsidians from the mediterranean area: a comparison with traditional XRF methods,” Archaeometry 50, 337–350. doi: 10.1111/j.1475-4754.2007.00355.x.Google Scholar
Eivindson, T. and Mikkelsen, O. (1999). Problems by using pressed powder pellets for XRF analysis of ferrosilicon alloys. ICPDS–International Centre for Diffraction Data.Google Scholar
Ellis, A. T. (2002). “Energy-Dispersive X-ray Fluorescence Analysis Using X-ray Tube Excitation,” in Handbook of X-Ray Spectrometry, 2nd ed, Revised and Expanded, edited by Van Grieken, R. E. and Markowicz, A. A. (Marcel Dekker, Inc., New York, USA).Google Scholar
Gaugliz, G. and Vo-Dinh, T. (Eds.) (2003). Handbook of Spectroscopy (Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim, Germany).Google Scholar
Goldstein, S. J., Slemmons, A. K., and Canavan, H. E. (1996). “Energy-dispersive X-ray fluorescence methods for environmental characterization of soils,” Environ. Sci. Technol., 30(7), 2318–2321.Google Scholar
Heckel, J. and Schramm, R. (1997). Bragg and Barkla polarization in EDXRF. ICPDS–International Centre for Diffraction Data. 40, 384–392.Google Scholar
Heckel, J., Haschke, M., Brumme, M., and Schindler, R. (1992). “Principles and applications of energy-dispersive X-ray fluorescence analysis with polarized radiation,” J. Anal. At. Spectrom., 7, 281–286.Google Scholar
Hicho, G. E. and Eaton, E. E. (1982). A Standard Reference Material Containing Nominally Five Percent Austenite (SRM 486a) (National Bureau of Standard Special Publication 260–76, Washington, USA).Google Scholar
Huber, L. (Ed.) (2010). Validation of Analytical Methods (Agilent Technologies, Germany).Google Scholar
Jenkin, R. (2000). “X-ray techniques: overview,” in Encyclopedia of Analytical Chemistry, edited by Meyers, R. A. (John Wiley & Sons Ltd, Chichester), pp. 13269–13288.Google Scholar
Jenkins, R. (Ed.) (1976). An Introduction to X-Ray Spectrometry (Heyden and Son Ltd., London, UK).Google Scholar
Jenkins, R. (Ed.) (1999). X-Ray Fluorescence Spectrometry (John Wiley & Sons Inc., USA), 2nd ed. pp. 189–197.CrossRefGoogle Scholar
Johnson, D. M., Hooper, P. R., and Conrey, R. M. (1999). XRF analysis of rocks and minerals for major and trace elements on a single low dilution Li-tetraborate fused bead. ICPDS–International Centre for Diffraction Data.Google Scholar
Kawahara, N. (2006). “Complex excitation effects and light elements”, In Handbook of Practical X-Ray Fluorescence Analysis, edited by Beckhoff, B., Kanngießer, B., Langhoff, N., Wedell, R., and Wolff, H. (Springer-Verlag, Berlin, Germany), pp. 379–384.Google Scholar
Larry, D. and Hanke, P. E. (Eds.) (2001). Handbook of Analytical Methods for Materials: Practical Solutions to Materials Problems through Technology and Innovation (Materials Evaluation and Engineering, Inc., Canada).Google Scholar
Leroy, C. and Rancoita, P. G. (Eds.) (2009). Principles of Radiation Interaction in Matter and Detection (World Scientific Publishing Co. Pte. Ltd., Singapore), 2nd ed., pp. 136–179.Google Scholar
Marguí, E., Queralt, I., Carvaiho, M. L., and Hidalgo, M. (2005). “Comparison of EDXRF and ICP-OES after microwave digestion for element determination in plant specimens from an abandoned mining area,” Anal. Chim. Acta, 549, 197–204.Google Scholar
Marguí, E., Queralt, I., and Hidalgo, M. (2009). “Application of x-ray fluorescence spectrometry to determination and quantitation of metals in vegetal material,” Trends Anal. Chem., 28(3), 362–372.Google Scholar
Miller, M. C. “X-ray fluorescence,” in Passive Nondestructive Assay of Nuclear Materials, edited by Reilly, D., Ensslin, N., Smith, H., and Kreiner, S. (Report NUREG/CR-5550, LA-UR-90-732, March 1991), Los Alamos, NM, USA, Los Alamos National Laboratory, Chapter 10, pp. 313–335.Google Scholar
Namowicz, C., Trentelman, K., and McGlinchey, C. (2009). “XRF of cultural heritage materials: round-robin IV – paint on canvas,” Powder Diffr. 24, 124–129.Google Scholar
Nielson, K. K., Mahoney, A. W., Williams, L. S., and Rogers, V. C. (1991). “X-ray fluorescence measurements of Mg, P, S, Cl, K, Ca, Mn, Fe, Cu, and Zn in fruits, vegetables, and grain products,” J. Food Compost. Anal. 4, 39–51.Google Scholar
Padilla, R., Van Espen, P., and Godo Torres, P. P. (2006). “The suitability of XRF analysis for compositional classification of archaeological ceramic fabric: a comparison with a previous NAA study,” Anal. Chim. Acta 558, 283–28. doi: 10.1016/j.aca.2005.10.077.Google Scholar
Schmeling, M., Van Grieken, R. E. (2002). “Sample Preparation for X-ray Fluorescence,” in Handbook of X-Ray Spectrometry, 2nd ed, Revised and Expanded, edited by Van Grieken, R. E. and Markowicz, A. A. (Marcel Dekker, Inc., New York, USA).Google Scholar
Schramm, R. and Heckel, J. (1998). “Fast analysis of traces and major elements with ED(P)XRF using polarized X-rays: TURBOQUANT,” J. Phys. IV Fr 8(P5), 335–342.Google Scholar
Schramm, R., Heckel, J., and Molt, K. (1999). ED(P)XRF: screening analysis and quantitative analysis with polarized X-rays. ICPDS–International Centre for Diffraction Data.Google Scholar
Shackley, M. S. (Ed.) (2011). X-Ray Fluorescence Spectrometry (XRF) in Geoarchaeology (Springer Science + Business Media, LLC, New York, USA). doi: 10.1007/978-1-4419-6886-9.Google Scholar
Tsoulfanidis, N. and Landsberger, S. (Eds.) (2011). Measurement and Detection of Radiation (CRC Press, Boca Raton, FL,USA), 3rd ed.Google Scholar
Van Meel, K., Smekens, A., Behets, M., Kazandjian, P., and Van Grieken, R. (2007). “Determination of platinum, palladium, and rhodium in automotive catalysts using high-energy secondary target X-ray fluorescence spectrometry,” Anal. Chem., 79(16), 6383–6389, doi: 10.1021/ac070815r.Google Scholar
Wien, K., Wissmann, D., Kölling, M., and Schulz, H. D. (2005). “Fast application of x-ray fluorescence spectrometry aboard ship: how good is the new portable Spectro Xepos analyser?,” Geo.-Mar. Lett. 25, 248–264, doi: 10.1007/s00367-004-0206-x.Google Scholar
Zschornack, G. (Ed.) (2007). Handbook of X-Ray Data (Springer-Verlag, Berlin, Germany).Google Scholar