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Impact of Sample Preparation on Mineralogical Analysis of Zero-Valent Iron Reactive Barrier Materials

D. H. Phillips*, B. Gu, D. B. Watson and Y. Roh

Environmental Sciences Division, Oak Ridge National Lab., P.O. Box 2008, Oak Ridge, TN 37831



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Fig. 1. Location of (a) angled cores in the Fe0 portion of the barrier and (b) vertical core through the whole Fe0 PRB. Figure not to scale.

 


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Fig. 2. Flowchart of the different mineralogical preparation treatments.

 


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Fig. 3. X-ray diffractograms showing the minerals present in different size fractions of acetone-dried, reduced loose core material (Samples 1 and 2a-1) (A, aragonite; C, calcite; F, zero-valent iron; GR, green rust; M, maghemite/magnetite; Q, quartz).

 


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Fig. 4. SEM micrographs of selected minerals (a) green rust, (b) siderite, (c) goethite with elongate aragonite crystals, and (d) aragonite from an unsieved whole sample. Arrows indicate points represented by EDX analysis (insets).

 


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Fig. 5. X-ray diffractograms showing the minerals present in samples analyzed at different times since sampling of the acetone-dried treatment on the reduced loose core material (Sample 2a-2) (A, aragonite; F, zero-valent iron; GR, green rusts; K, akaganeite; M, maghemite/magnetite; Q, quartz).

 


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Fig. 6. X-ray diffractograms showing the minerals present for samples analyzed at different times since sampling (T = 0 h and T = 11 d) of acetone-dried oxidized cemented core material (Sample 3) (A, aragonite; F, zero-valent iron; G, goethite; L, lepidocrocite; M, mackinawite; S, siderite; Q, quartz).

 


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Fig. 7. X-ray diffractograms showing the minerals present for the air-dried (25°C) and oven-dried (65 and 105°C) treatments of the reduced loose core material (Samples 2b–d) (A, aragonite; C, calcite; F, zero-valent iron; M, maghemite/magnetite; Q, quartz).

 





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