Journal of Soils and Sediments

, Volume 13, Issue 8, pp 1351–1359 | Cite as

Evaluation of soil analytical methods for the characterization of alkaline Technosols: II. Amorphous constituents and carbonates

  • Talitha C. Santini
  • Martin V. Fey
  • Michael N. Smirk



The aims of this study were to identify potential sources of error in common methods for determination of amorphous oxide concentrations and carbonate concentrations, as applied to a Technosolic material (bauxite residue), and where possible, suggest improvements to the methods.

Materials and methods

An acid ammonium oxalate (AAO) extraction was applied to fresh and weathered bauxite residues, at soil to solution ratios varying from 1:100 to 1:800. Two methods for carbonate concentration were compared: the ‘weight loss’ method, and the ‘difference in total C’ method. These were applied to six weathered bauxite residue samples, with CaCO3 concentrations ranging from 0.1–2 % weight.

Results and discussion

Chemically extractable amorphous content was underreported in bauxite residue at the standard 1:100 extraction ratio, likely due to Al and Si saturation of the oxalate complex. A 1:400 soil: AAO ratio extracted the highest amount of amorphous material. Some crystalline minerals such as sodalite, inherited from the Technosolic parent material, were soluble in the acid ammonium oxalate extractant. The difference in total C method was more precise than the weight loss method for the determination of carbonate concentration in bauxite residues.


The high amorphous content of bauxite residues requires a wider soil to solution ratio (1:400) for acid ammonium oxalate extraction than is used for typical soil materials (1:100). The difference in total C method is recommended for the routine analysis of field samples where small variations in carbonate concentration need to be detected.


Acid ammonium oxalate extraction Analytical methods Inorganic carbon Pedogenesis Tailings Technosols 



acid ammonium oxalate



The authors wish to thank Stephen Leavy and Kim-Louise Burke of Alcoa of Australia Limited. for assistance with ICPOES analyses; David Cooling, Patrick Keogh, and Keith Schmidt of Alcoa, Hezio Oliviera of Alumar, and Dianne McDonald of the Guyana Geology and Mines Commission for assisting with collection of bauxite residue samples; and Justin Kimpton, Helen Brand, and Qinfen Gu of the Australian Synchrotron for assistance with XRD analyses. Part of this research was undertaken on the Powder Diffraction (10BM1) beamline at the Australian Synchrotron, Victoria, Australia. Financial support for this work was provided by Alcoa of Australia Limited. and BHP Billiton Worsley Alumina, and a Minerals and Energy Research Institute of Western Australia scholarship to the senior author.


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Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Talitha C. Santini
    • 1
    • 2
  • Martin V. Fey
    • 1
  • Michael N. Smirk
    • 1
  1. 1.School of Earth and EnvironmentUniversity of Western AustraliaCrawleyAustralia
  2. 2.School of Geography and Earth SciencesMcMaster UniversityHamiltonCanada

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