Sample preparation method for characterization of fine solids in athabasca oil sands by electron microscopy

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DOIResolve DOI: http://doi.org/10.1021/ef200994a
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TypeArticle
Journal titleEnergy and Fuels
ISSN0887-0624
Volume25
Issue11
Pages51585164; # of pages: 7
SubjectAthabasca oil sands; Compositional information; Fine iron oxide; Fine particles; Fine solids; Flat surfaces; Focused ion beam technique; Hot water extraction; Low concentrations; Magnetite particles; Nano-sized; Polymer resins; Region of interest; Sample preparation methods; Scanning and transmission electron microscopy; SEM analysis; SEM image; Site-specific; TEM analysis; Thin section; X-ray mapping; X-ray maps; X-ray microanalysis; Electrons; Iron ores; Iron oxides; Oil sands; Sand; Solvent extraction; Transmission electron microscopy; X rays; X ray analysis
AbstractThis study introduces a new sample preparation method for characterization of fine solids in Athabasca oil sands using electron microscopy. The method uses a combination of microtome and focused ion beam (FIB) techniques to produce samples for both scanning and transmission electron microscopy (SEM/TEM). In this procedure, SEM images and X-ray maps provide general microstructure and compositional information, with detailed analysis provided through TEM analysis of site-specific electron transparent sections prepared using FIB methods. The method is particularly useful for identifying low concentrations of metals and their compounds and is demonstrated for the identification of fine iron oxide particles in the froth stream of an Athabasca oil sands sample after hot-water extraction. Fine particles (<2 μm fraction of oil sands minerals) are embedded in a polymer resin and sectioned using an ultramicrotome to prepare a fresh, flat surface for SEM analysis. An iron-rich region is located using X-ray mapping in the SEM. A thin section of the region of interest is prepared using FIB, which is then characterized using TEM imaging, electron diffraction, and X-ray microanalysis. Specifically, nanosized hematite and magnetite particles were identified in the froth stream. © 2011 American Chemical Society.
Publication date
LanguageEnglish
AffiliationNational Research Council Canada (NRC-CNRC); National Institute for Nanotechnology (NINT-INNT)
Peer reviewedYes
NPARC number21271465
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Record identifier1f89a5b7-204b-4ff6-a3b2-ccdfe3bad1ad
Record created2014-03-24
Record modified2016-05-09
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