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Journal of Soils and Sediments

, Volume 19, Issue 2, pp 830–839 | Cite as

Optimization of portable X-ray fluorescence spectrometry for the assessment of soil total copper concentrations: application at an ancient smelting site

  • Georgia Rogan
  • Matthew TigheEmail author
  • Peter Grave
  • Lisa Kealhofer
  • Pakpadee Yukongdi
  • Susan C. Wilson
Soils, Sec 4 • Ecotoxicology • Research Article

Abstract

Purpose

Copper (Cu) is the earliest anthropogenic metal pollutant, but knowledge of Cu soil concentrations at ancient metalworking sites is limited. The objective of this work was to examine the ability of portable X-ray fluorescence to quantify Cu in soils at such sites.

Materials and methods

Using a Bruker Tracer III-SD pXRF, we examine factory “scan” settings versus simple instrument parameter changes (a reduction in energy settings from 40 to 12 kV) to target analysis for Cu. We apply these to a set of uncontaminated samples (n = 18, < 92 mg Cu kg−1) from Central Thailand and compare results to standard wet chemistry analysis (aqua regia digestion and ICP-OES analysis). We then apply the optimized method to a set of highly contaminated samples (n = 86, < 14,200 mg Cu kg−1) from a known ancient smelting site.

Results and discussion

We demonstrate that simple changes to factory recommended “scan” settings can double the sensitivity of Cu determination via pXRF (“optimized limit of determination” of 19.3 mg kg−1 versus an initial value of 39.4 mg kg−1) and dramatically improve the accuracy of analysis. Changes to other results for other elements are variable and depend on concentration ranges, soil matrix effects, and pXRF response for the individual element. We demonstrate that pXRF can accurately determine Cu across a wide concentration range and identify grossly contaminated soil samples.

Conclusions

We conclude that pXRF is a useful tool to rapidly screen and analyse samples at remote sites and can be applied to ancient metalworking sites. Simple optimization of the pXRF settings greatly improves accuracy and is essential in determining comparative background concentrations and “unaffected” areas. Application to other elements requires further element and matrix specific optimization.

Keywords

Archaeometallurgy Pollution pXRF Soil Spectrometry 

Notes

Acknowledgements

This work was undertaken as part of a University of New England Research Seed Grant, and within an approved National Research Council of Thailand project (approval number 0002/1211). The authors would like to thank Dr. Fiorella Rispoli and Dr. Roberto Ciarla for site information and background, and Dr. Vince Piggott for discussions and project context.

Supplementary material

11368_2018_2091_MOESM1_ESM.docx (1.9 mb)
ESM 1 (DOCX 1923 kb)

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  1. 1.School of Environmental and Rural ScienceUniversity of New EnglandArmidaleAustralia
  2. 2.Archaeomaterials Science Hub, Archaeology and PalaeoanthropologyUniversity of New EnglandArmidaleAustralia
  3. 3.Anthropology and Environmental Studies and SciencesSanta Clara UniversitySanta ClaraUSA
  4. 4.Fine Arts DepartmentMinistry of CultureBangkokThailand

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