Development of an Affordable GD-OES Support Matrix for Analysis of Non-Conducting Zirconium Powders

Abstract:

Glow Discharge Optical Emission Spectroscopy (GD-OES) is an analytical technique mainly used in the analysis of solid metallic samples. The technique requires a conductive sample as the analyte serves as the cathode when generating the glow discharge plasma. GD-OES is useful for both bulk quantification and depth profiling of thin layers of conducting materials. The objective of this study was to develop a new sample support matrix for the preparation of conductive pressed pellets suitable for the analysis of non-conducting materials with GD-OES. In previous work non-conducting powders, such as uranium oxide, have been mixed with fine metal powders such as copper, silver or tantalum. Another solution has been to use a quick setting, conductive thermoplastic, such as diallyl phthalate impregnated with copper, as support. Both of these methods are, however, expensive and fairly time consuming. Graphite, a cheap, readily available conductive powder, proved not to form a strong enough pellet to withstand the conditions required during the GD analysis. This limitation was overcome by the addition of a binding agent, bakelite, to produce a relatively cheap, conductive matrix for the analysis of non-conducting powders. Spectroscopically pure zirconium oxide was used as a reference material and mixed with various quantities of graphite and bakelite powder. Two distinct regions of linearity were obtained. Samples with less than six percent zirconium yielded a gradient of 0.0011 with an R² value of 0.9949. Samples with higher zirconium content yielded a gradient of 0.0042 with an R² value of 0.9991. These results indicate the suitability of this sample matrix for analysis of zirconium materials by GD-OES.

• Periodical: Advanced Materials Research (Volume 1019)
• Pages: 393-397
• DOI: https://doi.org/10.4028/www.scientific.net/AMR.1019.393
• Online since: October 2014
• Authors: Steven James Lötter*, Walter Purcell, Johann T. Nel
• Keywords: GD-OES, Glow Discharge Optical Emission Spectroscopy, Graphite, Pressed Pellet, Zirconium

References

[1] Roskill Information Services Ltd, Zirconium: Global Industry Markets and Outlook, Thirteenth ed., London: Roskill Information Services Ltd, (2011).

DOI: 10.1093/ww/9780199540884.013.u175191

[2] R. E. Kirk and D. F. Othmer, Encyclopedia of Chemical Technology, Third ed., vol. 24, John Wiley and Sons, 1978, pp.863-896.

[3] W. B. Blumenthal, The Chemical Behaviour of Zirconium, New Jersey: D. Van Nostrand Company, (1958).

[4] ATI Wah Chang, ATI Metals, 2003. [Online]. Available: http: /www. atimetals. com/businesses/business-units/wahchang/products/Documents/Zr%20nuke%20waste%20disposal. pdf.

[5] Azom. com The A to Z of Materials, " 2 April 2004. [Online]. Available: http: /www. azom. com/article. aspx, ArticleID=2449. [Accessed 9 July 2013].

[6] K. Shimizu, H. Habazaki, P. Skeldon and G. E. Thompson, Impact of RF-GD-OES in practical surface analysis, Spectrochimica Acta Part B, vol. 58, pp.1573-1583, (2003).

DOI: 10.1016/s0584-8547(03)00133-2

[7] A. Bogaerts and R. Gijbels, Fundamental aspects and applications of glow discharge spectrometric techniques, Spectrochimica Acta Part B, vol. 53, pp.1-42, (1998).

DOI: 10.1016/s0584-8547(97)00122-5

[8] M. Betti, Use of a Direct Current Glow Discharge Mass Spectrometer for the Chemical Characterization of Samples of Nuclear Concern, Journal of Analytical Atomic Spectrometry, vol. 11, pp.855-860, (1996).

DOI: 10.1039/ja9961100855

[9] I. Kenawy, Untersuchungen zur emissionsspeltroslopischen Bestimmung der Halogene und Chalkogene in nichtmetallischen Proben mit Hilfe von Glimmentladungen, Bochum: der Ruhr-Universitat Bochum, 1980, p.146.