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Journal of Environmental Quality 32:1299-1305 (2003)
© 2003 American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America

TECHNICAL REPORTS
Ground Water Quality

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

* Corresponding author (dhphillips2003{at}yahoo.com)

Received for publication March 11, 2002. Permeable reactive barriers (PRBs) of zero-valent iron (Fe0) are increasingly being used to remediate contaminated ground water. Corrosion of Fe0 filings and the formation of precipitates can occur when the PRB material comes in contact with ground water and may reduce the lifespan and effectiveness of the barrier. At present, there are no routine procedures for preparing and analyzing the mineral precipitates from Fe0 PRB material. These procedures are needed because mineralogical composition of corrosion products used to interpret the barrier processes can change with iron oxidation and sample preparation. The objectives of this study were (i) to investigate a method of preparing Fe0 reactive barrier material for mineralogical analysis by X-ray diffraction (XRD), and (ii) to identify Fe mineral phases and rates of transformations induced by different mineralogical preparation techniques. Materials from an in situ Fe0 PRB were collected by undisturbed coring and processed for XRD analysis after different times since sampling for three size fractions and by various drying treatments. We found that whole-sample preparation for analysis was necessary because mineral precipitates occurred within the PRB material in different size fractions of the samples. Green rusts quickly disappeared from acetone-dried samples and were not present in air-dried and oven-dried samples. Maghemite/magnetite content increased over time and in oven-dried samples, especially after heating to 105°C. We conclude that care must be taken during sample preparation of Fe0 PRB material, especially for detection of green rusts, to ensure accurate identification of minerals present within the barrier system.

Abbreviations: Fe0, zero-valent iron • PRB, permeable reactive barrier • XRD, X-ray diffraction


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JEQ 2003 32: 1167-1172. [Full Text]  



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J. Environ. Qual., March 1, 2005; 34(2): 487 - 495.
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J. Environ. Qual.Home page
D. H. Phillips, D. B. Watson, Y. Roh, and B. Gu
Mineralogical Characteristics and Transformations during Long-Term Operation of a Zerovalent Iron Reactive Barrier
J. Environ. Qual., November 1, 2003; 32(6): 2033 - 2045.
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