Skip to main content
SpringerLink
Log in

Recovery of iron/iron oxide nanoparticles from solution: comparison of methods and their effects

  • Research Paper
  • Published:
Journal of Nanoparticle Research Aims and scope Submit manuscript

Abstract

Most methods currently being used to recover Fe0-core/oxide-shell nanoparticles from solutions (including the solvents they are synthesized or stored in) are potentially problematic because they may alter the particle composition (e.g., depositing salts formed from solutes) or leave the particles prone to transformations during subsequent storage and handling (e.g., due to residual moisture). In this study, several methods for recovery of nanoparticles from aqueous solution were studied to determine how they affect the structure and reactivity of the recovered materials. Simple washing of the nanoparticles during vacuum filtration (i.e., “flash drying”) can leave up to ~17 wt% residual moisture. Modeling calculations suggest this moisture is mostly capillary or matric water held between particles and particle aggregates, which can be removed by drying for short periods at relative vapor pressures below 0.9. Flash drying followed by vacuum drying, all under N2, leaves no detectable residue from precipitation of solutes (detectable by X-ray photoelectron spectroscopy, XPS), no significant changes in overall particle composition or structure (determined by transmission electron microscopy, TEM), and negligible residual moisture (by thermogravimetric analysis, TGA). While this improved flash-drying protocol may be the preferred method for recovering nanoparticles for many purposes, we found that Fe0-core/oxide-shell nanoparticles still exhibit gradual aging during storage when characterized electrochemically with voltammetry.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10
Fig. 11
Fig. 12
Fig. 13
Fig. 14

Similar content being viewed by others

References

  • Anderson JF, Kuhn M, Diebold U (1998) Epitaxially grown Fe3O4 thin films: an XPS study. Surf. Sci. Spectra 4:266–272

    Article  Google Scholar 

  • Baer DR, Tratnyek PG, Qiang Y, Amonette JE, Linehan J, Sarathy V, Nurmi JT, Wang C, Anthony J (2007) Synthesis, characterization, and properties of zero-valent iron nanoparticles. In: Fryxell GE (ed) Environmental applications of nanomaterials: synthesis, sorbents, and sensors. Imperial College Press, London, pp 49–86

    Chapter  Google Scholar 

  • Baer DR, Amonette JE, Engelhard MH, Gaspar DJ, Karakoti AS, Kuchibhatla S, Nachimuthu P, Nurmi JT, Qiang Y, Sarathy V, Seal S, Sharma A, Tratnyek PG, Wang C-M (2008) Characterization challenges for nanomaterials. Surf. Interface Anal. 40:529–537

    Article  CAS  Google Scholar 

  • Bordia RK (1984) A theoretical analysis of random packing densities of mono-sized spheres in two and three dimensions. Scr Metall Mater 18:725–730

    CAS  Google Scholar 

  • Burleson DJ, Driessen MD, Penn RL (2004) On the characterization of environmental nanoparticles. J Environ Sci Health A 39:2707–2753

    Article  Google Scholar 

  • Cao X, Koltypin Y, Kataby G, Prozorov R, Gedanken A (1995) Controlling the particle size of amorphous iron nanoparticles. J Mater Res 10:2952–2957

    Article  CAS  Google Scholar 

  • Chambers SA, Kim YJ, Gao Y (1998) Fe 2p Core-level spectra for pure, epitaxial α-Fe2O3(0001), γ-Fe2O3(001), and Fe3O4(001). Surf Sci Spectra 5:219–228

    Article  CAS  Google Scholar 

  • Chin AB, Yaacob II (2006) Synthesis and characterization of iron oxides nanoparticles. Key Eng Mater 306–308:1115–1119

    Article  Google Scholar 

  • European Network on the Health and Environmental Impact of Nanomaterials (2008) NanoImpactNet workshop 1—strategies to standardize nanomaterials for environmental and ecotoxicological research (3–5 September 2008, Zurich, Switzerland)

  • Gaspar DJ, Engelhard MH, Henry MC, Baer DR (2005) Erosion rate variations during XPS sputter depth profiling of nanoporous films. Surf Interface Anal 37:417–423

    Article  CAS  Google Scholar 

  • Grainger DW, Castner DG (2008) Nanobiomaterials and nanoanalysis: opportunities for improving the science to benefit biomedical technologies. Adv Mater 20:867–877

    Article  CAS  Google Scholar 

  • Grosvenor AP, Kobe BA, McIntyre NS (2004) Studies of the oxidation of iron by water vapour using X-ray photoelectron spectroscopy and QUASES. Surf Sci 572:217–227

    Article  CAS  Google Scholar 

  • Jia X, Gan M, Williams RA, Rhodes D (2007) Validation of a digital packing algorithm in predicting powder packing densities. Powder Technol 174:10–13

    Article  CAS  Google Scholar 

  • Johnson RL, O’Brien Johnson R, Nurmi JT, Tratnyek PG (2009) Natural organic matter enhanced mobility of nano zero-valent iron. Environ Sci Technol 43:5455–5460

    Article  CAS  Google Scholar 

  • Kim J-H, Tratnyek PG, Chang Y-S (2008) Rapid dechlorination of polychlorinated dibenzo-p-dioxins (PCDDs) by bimetallic and nano-sized zerovalent iron. Environ Sci Technol 42:4106–4112

    Article  CAS  Google Scholar 

  • Klabunde KJ (2001) Nanoscale materials in chemistry. Wiley, New York

    Book  Google Scholar 

  • Li L, Fan M, Brown R, Van Leeuwen J, Wang J, Wang W, Song Y, Zhang P (2006a) Synthesis, properties, and environmental applications of nanoscale iron-based materials: a review. Crit Rev Environ Sci Technol 36:405–431

    Article  CAS  Google Scholar 

  • Li X-Q, Elliott DW, Zhang W-X (2006b) Zero-valent iron nanoparticles for abatement of environmental pollutants: materials and engineering aspects. Crit Rev Solid State Mater Sci 31:111–122

    Article  CAS  Google Scholar 

  • Lienemann C-P, Heissenberger A, Leppard GG, Perret D (1998) Optimal preparation of water samples for the examination of colloidal materials by transmission electron microscopy. Aquat Microb Ecol 14:205–213

    Article  Google Scholar 

  • Liu Y, Lowry GV (2006) Effect of particle age (Fe0 content) and solution pH on nZVI reactivity: H2 evolution and TCE dechlorination. Environ Sci Technol 40:6085–6090

    Article  CAS  Google Scholar 

  • Liu Y, Majetich Sara A, Tilton Robert D, Sholl David S, Lowry Gregory V (2005) TCE dechlorination rates, pathways, and efficiency of nanoscale iron particles with different properties. Environ Sci Technol 39:1338–1345

    Article  CAS  Google Scholar 

  • Lowry GV, Johnson KM (2004) Congener-specific dechlorination of dissolved PCBs by microscale and nanoscale zerovalent iron in a water/methanol solution. Environ Sci Technol 38:5208–5216

    Article  CAS  Google Scholar 

  • Moulder JF, Stickle WF, Sobol PE, Bomben KD (eds) (1992) Handbook of X-ray photoelectron spectroscopy. Perkin-Elmer Corp, Eden Prairie, MN

    Google Scholar 

  • National Institute of Standards and Technology (2008) ISO, IEC, NIST, and OECD international workshop on documentary standards for measurement and characterization of nanotechnologies (26–28 February 2008)

  • Nurmi JT, Tratnyek PG (2008) Electrochemical studies of packed iron powder electrodes: effects of common constituents of natural waters on corrosion potential. Corros Sci 50:144–154

    Article  CAS  Google Scholar 

  • Nurmi JT, Bandstra JZ, Tratnyek PG (2004) Packed powder electrodes for characterizing the reactivity of granular iron in borate solutions. J Electrochem Soc 151:B347–B353

    Article  CAS  Google Scholar 

  • Nurmi JT, Tratnyek PG, Sarathy V, Baer DR, Amonette JE, Pecher K, Wang C, Linehan JC, Matson DW, Penn RL, Driessen MD (2005) Characterization and properties of metallic iron nanoparticles: spectroscopy, electrochemistry, and kinetics. Environ Sci Technol 39:1221–1230

    Article  CAS  Google Scholar 

  • Obare SO, Meyer GJ (2004) Nanostructured materials for environmental remediation of organic contaminants in water. J Environ Sci Health A 39:2549–2582

    Article  Google Scholar 

  • Perret D, Leppard GG, Mueller M, Belzile N, De Vitre R, Buffle J (1991) Electron microscopy of aquatic colloids: non-perturbing preparation of specimens in the field. Water Res 25:1333–1343

    Article  CAS  Google Scholar 

  • Reardon EJ, Fagan R, Vogan JL, Przepiora A (2008) Anaerobic corrosion reaction kinetics of nano-sized iron. Environ Sci Technol 42:2420–2425

    Article  CAS  Google Scholar 

  • Rose J, Thill A, Brant J (2007) Methods of structural and chemical characterization of nanomaterials. In: Wiesner MR, Bottero J-Y (eds) Environmental nanotechnology. McGraw Hill, New York, pp 105–154

    Google Scholar 

  • Sarathy V, Tratnyek PG, Nurmi JT, Baer DR, Amonette JE, Chun C, Penn RL, Reardon EJ (2008) Aging of iron nanoparticles in aqueous solution: effects on structure and reactivity. J Phys Chem C 112:2286–2293

    Article  CAS  Google Scholar 

  • Song H, Carraway ER (2005) Reduction of chlorinated ethanes by nanosized zero-valent iron: kinetics, pathways, and effects of reaction conditions. Environ Sci Technol 39:6237–6245

    Article  CAS  Google Scholar 

  • Song H, Carraway ER (2006) Reduction of chlorinated methanes by nano-sized zero-valent iron: kinetics, pathways, and effect of reaction conditions. Environ Eng Sci 23:272–284

    Article  CAS  Google Scholar 

  • Song H, Carraway ER (2008) Catalytic hydrodechlorination of chlorinated ethenes by nanoscale zero-valent iron. Appl Catal B 78:53–60

    Article  CAS  Google Scholar 

  • Sun Y-P, Li X-Q, Cao J, Zhang W-X, Wang HP (2006) Characterization of zero-valent iron nanoparticles. Adv Colloid Interface Sci 120:47–56

    Article  CAS  Google Scholar 

  • Sweeney SF, Woehrle GH, Hutchison JE (2006) Rapid purification and size separation of gold nanoparticles via diafiltration. J Am Chem Soc 128:3190–3197

    Article  CAS  Google Scholar 

  • Tratnyek PG, Johnson RL (2006) Nanotechnologies for environmental cleanup. NanoToday 1:44–48

    Google Scholar 

  • Uegami M, Kawano J, Okita T, Fujii Y, Okinaka K, Kakuya K, Yatagai S (2007) Process for purifying contaminated soil or groundwater with iron particles. Toda Kogyo Corp., United States Patent, No. 7,220,366 B2

  • Wiesner MR, Lowry GV, Alvarez P, Dionysiou D, Biswas P (2006) Assessing the risks of manufactured nanomaterials. Environ Sci Technol 40:4336–4345

    Article  CAS  Google Scholar 

  • Zhang H, Gilbert B, Huang F, Banfield JF (2003) Water-driven structure transformation in nanoparticles at room temperature. Nature 424:1025–1029

    Article  CAS  Google Scholar 

Download references

Acknowledgments

We acknowledge and thank C.-M. Wang, P. Nachimuthu, M.H. Engelhard, J. Kwak, and C.K. Russell for their assistance with TEM, XRD, XPS, and BET measurements and sample preparation. Samples of nano-Fe0 were donated by the Toda Kogyo Corp. We would also like to thank students Abram J. Ledbetter and Jharana Dhal who conducted some exploratory work on particle recovery during a Nanotechnology course hosted by the Pacific Northwest National Laboratory (PNNL) and the William R. Wiley Environmental Molecular Sciences Laboratory (EMSL). This work was supported by the U.S. Department of Energy (DOE) Division of Chemical Sciences, Geosciences, and Biosciences. Parts of the work were conducted at the EMSL, which is located at PNNL. EMSL is a DOE User Facility operated by Battelle for the DOE Office of Biological and Environmental Research. PNNL is operated for the DOE under Contract DE-AC06-76RLO 1830.

Author information

Authors and Affiliations

  1. Division of Environmental and Biomolecular Systems, Oregon Health & Science University, 20000 NW Walker Road, Portland, OR, 97006, USA

    James T. Nurmi, Vaishnavi Sarathy & Paul G. Tratnyek

  2. Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Box 999, Richland, WA, 99352, USA

    Donald R. Baer

  3. Fundamental and Computational Sciences Directorate, Pacific Northwest National Laboratory, Box 999, Richland, WA, 99352, USA

    James E. Amonette & Abhi Karkamkar

Authors
  1. James T. Nurmi
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Vaishnavi Sarathy
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Paul G. Tratnyek
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Donald R. Baer
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. James E. Amonette
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Abhi Karkamkar
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding authors

Correspondence to Paul G. Tratnyek or Donald R. Baer.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Nurmi, J.T., Sarathy, V., Tratnyek, P.G. et al. Recovery of iron/iron oxide nanoparticles from solution: comparison of methods and their effects. J Nanopart Res 13, 1937–1952 (2011). https://doi.org/10.1007/s11051-010-9946-x

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11051-010-9946-x

Keywords

Search

Navigation