Evaluation of Characterization Techniques for Iron Pipe Corrosion Products and Iron Oxide Thin Films
Publication: Journal of Environmental Engineering
Volume 134, Issue 10
Abstract
A common problem faced by drinking water studies is that of properly characterizing the corrosion products (CP) in iron pipes or synthetic Fe (hydr)oxides used to simulate the iron pipe used in municipal drinking-water systems. The present work compares the relative applicability of a suite of imaging and analytical techniques for the characterization of CPs and synthetic Fe oxide thin films and provide an overview of the type of data that each instrument can provide as well as their limitations to help researchers and consultants choose the best technique for a given task. Crushed CP from a water distribution system and synthetic Fe oxide thin films formed on glass surfaces were chosen as test samples for this evaluation. The CP and synthetic Fe oxide thin films were analyzed by atomic force microscopy (AFM), scanning electron microscopy (SEM), energy-dispersive spectroscopy, time-of-flight secondary ion mass spectrometry (ToF-SIMS), X-ray powder diffractometry (XRD), grazing incident diffractometry (GID), transmission electron microscopy (TEM), selected area electron diffraction, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared, Mössbauer spectroscopy, Brunauer–Emmett–Teller adsorption and Fe concentration was determined by the ferrozine method. XRD and GID were found to be the most suitable techniques for identification of the mineralogical composition of CP and synthetic Fe oxide thin films, respectively. AFM and a combined ToF-SIMS–AFM approach proved excellent for roughness and depth profiling analysis of synthetic Fe oxide thin films, respectively. Corrosion products were difficult to study by AFM due to their surface roughness, while synthetic Fe oxide thin films resisted most spectroscopic methods due to their limited thickness . XPS analysis is not recommended for mixtures of Fe (hydr)oxides due to their spectral similarities. SEM and TEM provided great detail on mineralogical morphology.
Get full access to this article
View all available purchase options and get full access to this article.
Acknowledgments
Analytical work was performed at the Image and Chemical Analysis Laboratory at Montana State University (MSU) and the W. R. Wiley Environmental Molecular Sciences Laboratory (EMSL) at Pacific Northwest National Laboratory, operated for the Department of EnergyDOE by Battelle. Special thanks go to Alice Dohnalkova, Ravi Kukkadapu, and David McCready at EMSL for their scientific and technical contributions. Support was provided by Colorado State University to the lead writer, the U. S. Department of Defense, Army Research Office, Grant No. DDREDAAD19-99-1-0092, the USEPA through its Office of Research and Development partially funded and collaborated in this research under Agreement No. UNSPECIFIEDCR-826927010, and this research was also partially supported by the U.S. Department of Energy, Office of Science, Environmental Management Science Program, under Grant No. DOEDE-FG02-03ER63582. The writers also acknowledge the thoughtful comments provided by the associate editor and four anonymous reviewers.
References
American Water Works Association (AWWA). (1996). Internal corrosion of water distribution systems, 2nd Ed., AWWA Research Foundation, Denver.
American Water Works Association (AWWA). (2003). “Type of pipe material in place for water distribution.” AWWA MainStream, Vol. 47, 1, American Water Works Association, Denver.
Appenzeller, B. M. R., Duval, Y. B., Thomas, F., and Block, J. (2002). “Influence of phosphate on bacterial adhesion onto oxyhydroxide in drinking water.” Environ. Sci. Technol., 36, 646–652.
Arce, F. T., Avci, R., Beech, I. B., Cooksey, K. E., and Wigglesworth-Cooksey, B. (2003). “Microelastic properties of minimally adhesive surfaces: A comparative study of RTV11TM and Intersleek elastomers™.” J. Chem. Phys., 119(3), 1671–1682.
Benjamin, M. M., Sletten, R. S., and Bailey, R. P. (1996). “Sorption and filtration of metals using iron-oxide-coated sand.” Water Res., 30, 2609–2620.
Borch, T., Masue, Y., Kukkadapu, R. K., and Fendorf, S. (2007). “Phosphate imposed limitations on biological reduction and alteration of ferrihydrite.” Environ. Sci. Technol., 41(1), 166–172.
Butterfield, P. W., Camper, A. K., Biederman, J. A., and Bargmeyer, A. M. (2002). “Minimizing biofilm in the presence of iron oxides and humic substances.” Water Res., 36, 3898–3910.
Chang, Y. J., Li, C. W., and Benjamin, M. M. (1997). “Iron oxide-coated media for NOM sorption and particulate filtration.” J. Am. Water Works Assoc., 89(5), 100–113.
Cheng, Z. Q., Van Geen, A., Jing, C. Y., Meng, X. G., Seddique, A., and Ahmed, K. M. (2004). “Performance of a household-level arsenic removal system during deployments in Bangladesh.” Environ. Sci. Technol., 38(12), 3442–3448.
Chun, C. L., Hozalski, R. M., and Arnold, T. A. (2005). “Degradation of drinking water disinfection byproducts by synthetic goethite and magnetite.” Environ. Sci. Technol., 39(21), 8525–8532.
Chun, C. L., Hozalski, R. M., and Arnold, W. A. (2007). “Degradation of disinfection byproducts by carbonate green rust.” Environ. Sci. Technol., 41(5), 1615–1621.
Cook, D. C. (2004). “Application of Mossbauer spectroscopy to the study of corrosion.” Hyperfine Interact., 153(1–4), 61–82.
Cornell, R. M., and Schwertmann, U. (1996). The iron oxides, VCH, New York.
Dong, H., Fredrickson, J. K., Kennedy, D. W., Zachara, J. M., Kukkadapu, R. K., and Onstott, T. C. (2000). “Mineral transformation associated with the microbial reduction of magnetite.” Chem. Geol., 169, 299–318.
Godelitsas, A., Astilleros, J. M., Hallam, K., Harissopoulos, S., and Putnis, A. (2003). “Interaction of calcium carbonates with lead in aqueous solutions.” Environ. Sci. Technol., 37(15), 3351–3360.
Hansen, B. O., Kwan, P., Benjamin, M. M., Li, C., and Korshin, G. V. (2001). “Use of iron oxide-coated sand to remove strontium from simulated Hanford tank wastes.” Environ. Sci. Technol., 35, 4905–4909.
Instruments, D. (1997). DimensionTM 3100 instruction manual, Santa Barbara, Calif.
Joshi, A., and Chaudhuri, M. (1996). “Removal of arsenic from ground water by iron oxide-coated sand.” J. Environ. Eng., 122, 769–771.
Kazi, Z. A. H., Kevin, C. B., and Christopher, M. M. (2006). “Iron oxide enhanced chlorine decay and disinfection by-product formation.” J. Environ. Eng., 132(12), 1609–1616.
Korshin, G. V., Benjamin, M. M., and Sletten, R. S. (1997). “Adsorption of natural organic matter (NOM) on iron oxide: Effects on NOM composition and formation of organo-halide compounds during chlorination.” Water Res., 31(7), 1643–1650.
Kosaka, T., Suzuki, S., Inoue, H., Saito, M., Waseda, Y., and Matsubara, E. (1995). “XPS/GIXS studies of thin oxide films formed on Fe-Cr alloys.” Appl. Surf. Sci., 103, 55–61.
Kukkadapu, R. K., Zachara, J. M., Fredrickson, J. K., and Kennedy, D. W. (2004). “Biotransformation of two-line silica-ferrihydrite by a dissimilatory Fe(III)-reducing bacterium: Formation of carbonate green rust in the presence of phosphate.” Geochim. Cosmochim. Acta, 68(13), 2799–2814.
Lai, C. H., and Chen, C. Y. (2001). “Removal of metal ions and humic acid from water by iron-coated filter media.” Chemosphere, 44(5), 1177–1184.
LeChevallier, M. W., Welch, N. J., and Smith, D. B. (1996). “Full scale studies of factors related to coliform regrowth in drinking water.” Appl. Environ. Microbiol., 62, 2201–2211.
Lin, J., Ellaway, M., and Adrien, R. (2001). “Study of corrosion material accumulated on the inner wall of steel water pipe.” Corros. Sci., 43(11), 2065–2081.
McIntyre, N. S., and Zetaruk, D. G. (1977). “X-ray photoelectron spectroscopic studies of iron oxides.” Anal. Chem., 49(11), 1521–1529.
McNeill, L. S., and Edwards, M. (2001). “Iron pipe corrosion in distribution systems.” J. Am. Water Works Assoc., 93(7), 88–100.
Murad, E., and Schwertmann, U. (1980). “The Mossbauer spectrum of ferrihydrite and its relations to those of other iron-oxides.” Am. Mineral., 65(9–10), 1044–1049.
National Research Council (NRC). (2006). Drinking water distribution systems: Assessing and reducing risk, National Academies Press, Washington, D.C.
O’Day, P. A., Rivera, N., Root, R., and Carroll, S. A. (2004). “X-ray absorption spectroscopic study of Fe reference compounds for the analysis of natural sediments.” Am. Mineral., 89(4), 572–585.
O’Loughlin, E. J., Kemner, K. M., and Burris, D. R. (2003). “Effects of Ag(I), Au(III), and Cu(II) on the reductive dechlorination of carbon tetrachloride by green rust.” Environ. Sci. Technol., 37(13), 2905–2912.
Parsons, J. G., Aldrich, M. V., and Gardea-Torresdey, J. L. (2002). “Environmental and biological applications of extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge structure (XANES) spectroscopies.” Appl. Spectrosc. Rev., 37(2), 187–222.
Perret, D., Gaillard, J., Dominik, J., and Atteia, O. (2000). “The diversity of natural hydrous iron oxides.” Environ. Sci. Technol., 34, 3540–3546.
Peulon, S., Legrand, L., Antony, H., and Chausse, A. (2003). “Electrochemical deposition of thin films of green rusts 1 and 2 on inert gold substrate.” Electrochem. Commun., 5(3), 208–213.
Refait, P., Memet, J.-B., Bon, C., Sabot, R., and Genin, J.-M. R. (2003). “Formation of the Fe(II)-Fe(III) hydroxysulphate green rust during marine corrosion of steel.” Corros. Sci., 45(4), 833–845.
Rieke, P. C., Marsh, B. D., Wood, L. L., Tarasevich, B. J., Liu, J., and Fryxell, G. E. (1995). “Aqueous solution deposition kinetics of iron oxyhydroxide on sulfonic acid terminated self-assembled monolayers.” Langmuir, 11, 318–326.
Russel, P., Batchelor, D., and Thornton, J. (2003). “Scanning electron microscopy (SEM) and atomic force microscopy (AFM): Complementary techniques for high resolution surface investigations.” ⟨www.di.com⟩, 1–12.
Sarin, P., Snoeyink, V. L., Bebee, J., Kriven, W. M., and Clement, J. A. (2001). “Physico-chemical characteristics of corrosion scales in old iron pipes.” Water Res., 35(12), 2961–2969.
Sarin, P., Snoeyink, V. L., Lytle, D. A., and Kriven, W. M. (2004). “Iron corrosion scales: Model for scale growth, iron release, and colored water formation.” J. Environ. Eng., 130(4), 364–373.
Scheidegger, A., Borkovec, M., and Sticher, H. (1993). “Coating of silica sand with goethite: Preparation and analytical identification.” Geoderma, 58, 43–65.
Scheinost, A. C., Chavernas, A., Barron, V., and Torrent, J. (1998). “Use and limitations of second-derivative diffuse reflectance spectroscopy in the visible to near-infrared range to identify and quantify Fe oxide minerals in soils.” Clays Clay Miner., 46(5), 528–536.
Shellenberger, K., and Logan, B. E. (2002). “Effect of molecular scale roughness of glass beads on colloidal and bacterial deposition.” Environ. Sci. Technol., 36, 184–189.
Smith, S. E., Bisset, A., Colbourne, J. S., Holt, D., and Lloyd, B. J. (1997). “The occurrence and significance of particles and deposits in a drinking water distribution system.” J. N. Engl. Water Works Assoc., 111, 135–150.
Solozhenkin, P., Zouboulis, A., and Katsoyiannis, I. (2007). “Removal of arsenic compounds from waste water by chemisorption filtration.” Theor. Found. Chem. Eng., 41(5), 772–779.
Stenkamp, V. S., and Benjamin, M. M. (1994). “Effect of iron oxide coating on sand filtration.” New Sci., 83, 37–50.
Szabo, J. G., Rice, E. W., and Bishop, P. L. (2007). “Persistence and decontamination of Bacillus atrophaeus subsp. globigii spores on corroded iron in a model drinking water system.” Appl. Environ. Microbiol., 73(8), 2451–2457.
Thirunavukkarasu, O. S., Viraraghavan, T., and Subramanian, K. S. (2001). “Removal of arsenic in drinking water by iron oxide-coated sand and ferrihydrite-batch studies.” Water Qual. Res. J. Canada, 36(1), 55–70.
Vertes, A., and Czakonagy, I. (1989). “Mossbauer-spectroscopy and its application to corrosion studies.” Electrochim. Acta, 34(6), 721–758.
Vikesland, P. J., and Valentine, R. L. (2002). “Iron oxide surface-catalyzed oxidation of ferrous iron by monochloramine: Implications of oxide type and carbonate on reactivity.” Environ. Sci. Technol., 36(3), 512–519.
Williams, M. M., and Braun-Howland, E. B. (2003). “Growth of escherichia coli in model distribution system biofilms exposed to hypochlorous acid or monochloramine.” Appl. Environ. Microbiol., 69(9), 5463–5471.
Information & Authors
Information
Published In
Journal of Environmental Engineering
Volume 134 • Issue 10 • October 2008
Pages: 835 - 844
Copyright
© 2008 ASCE.
History
Received: Dec 4, 2007
Accepted: Feb 27, 2008
Published online: Oct 1, 2008
Published in print: Oct 2008
Authors
Metrics & Citations
Metrics
Citations
Download citation
If you have the appropriate software installed, you can download article citation data to the citation manager of your choice. Simply select your manager software from the list below and click Download.