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Experimental Study of Tio2 Nanoparticle Adhesion to Silica and Fe(III) Oxide-Coated Silica Surfaces

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Experimental Study of Tio2 Nanoparticle Adhesion to Silica and Fe(III) Oxide-Coated Silica Surfaces Chemical Geology 332–333 (2012) 148–156 Contents lists available at SciVerse ScienceDirect Chemical Geology journal homepage: www.elsevier.com/locate/chemgeo Experimental study of TiO2 nanoparticle adhesion to silica and Fe(III) oxide-coated silica surfaces Lindsay A. Seders Dietrich a,⁎, Manoranjan Sahu b,1, Pratim Biswas b, Jeremy B. Fein a a University of Notre Dame, Department of Civil & Environmental Engineering & Earth Sciences, Notre Dame, IN 46556, USA b Washington University in St. Louis, Department of Energy, Environmental and Chemical Engineering, St. Louis, MO 63130, USA article info abstract Article history: With the rapid expansion of industrial nanotechnology applications, engineered nanoparticles are being in- Received 8 June 2012 troduced into the environment before the controls on their fate and mobility are fully understood. In this Received in revised form 7 September 2012 study, we measured the adhesion of TiO2 nanoparticles onto silica and Fe(III) oxide-coated silica surfaces Accepted 14 September 2012 as a function of pH, nanoparticle concentration, and nanoparticle size. Batch TiO adhesion experiments Available online 4 October 2012 2 were conducted at pH 3–8 and 0.01 M NaClO4 with TiO2 concentrations ranging from 10 to 200 mg/L. Editor: B. Sherwood Lollar Three TiO2 size fractions, each containing a range of particle sizes, had initial average diameters of 16, 26, and 50 nm. Silica grains, both uncoated and coated with Fe(III) oxide, were used as the geosorbents. The ex- Keywords: tent of TiO2 nanoparticle adhesion increased with increasing nanoparticle concentration, and pH exerted a Titanium dioxide nanoparticle strong effect on the adhesion behavior of the nanoparticles onto the uncoated silica particles. At and below Adhesion pH 5, TiO2 nanoparticle adhesion increased with increasing pH; at pH 6 and above, adhesion occurred inde- Silica pendently of pH. In general, the differences in adhesion between the three nanoparticle sizes at a given pH Iron oxide coating were not large. Within a given size fraction, preferential adhesion of the larger TiO2 particles was suggested below pH 6, and preferential adhesion of the smaller TiO2 particles was suggested at and above pH 6. Exper- iments with the Fe-coated silica grains were conducted only with the 26 nm TiO2 nanoparticles, and, except at pH 6 where we observed significantly enhanced adhesion to the Fe-coated silica relative to the uncoated silica, the extents of nanoparticle adhesion onto the two geosorbents were the same within experimental un- certainty. The similarity in adhesion behaviors onto solids with such different surface chemistries suggests that the properties of the TiO2 nanoparticles, such as agglomeration, and not of the mineral surfaces, are pri- marily responsible for governing adhesion. © 2012 Elsevier B.V. All rights reserved. 1. Introduction potentially detrimental in environmental systems where unwanted in- hibition of bacterial growth has been shown to occur (Adams et al., In recent years, the use of engineered nanoparticles has expanded 2006). In addition, exposure to nano-sized TiO2 particles may be toxic rapidly into a variety of industries, and many consumer products rang- (Long et al., 2006; Nel et al., 2006; Wiesner et al., 2006; Limbach et al., ing from shampoo and cosmetics to tires and tennis racquets now con- 2007; Wang et al., 2007; Simon-Deckers et al., 2008; Brunet et al., tain nanoparticles (Wiesner et al., 2006). Titanium dioxide (TiO2) 2009). However, despite their widespread industrial use and potential nanoparticles are especially common in a number of products and are release into the environment, the controls on the fate and mobility of being introduced into aquatic and subsurface geologic systems either TiO2 nanoparticles in the subsurface have not been well characterized. inadvertently, such as through the weathering of exterior paint (Kaegi Both agglomeration and surface adhesion can affect the mobility et al., 2008), or intentionally as a tool for environmental remediation of engineered nanoparticles in geologic systems. Most previous re- (e.g., Mattigod et al., 2005; Pena et al., 2005; Theron et al., 2008; search has focused on agglomeration processes, demonstrating the Oyama et al., 2009). TiO2 nanoparticles exhibit antibacterial properties, prevalence of TiO2 nanoparticle agglomerates under a wide range which may be beneficial in pharmaceutical applications but are of aqueous conditions and with nanoparticles of many sizes (Lecoanet et al., 2004; Dunphy Guzman et al., 2006; Ridley et al., ⁎ Corresponding author at: Department of Civil and Environmental Engineering, 2006; Choy et al., 2008; Domingos et al., 2009; Fatisson et al., 2009; Southern Methodist University, P.O. Box 750340, Dallas, TX 75275-0340, USA. Tel.: +1 French et al., 2009; Jiang et al., 2009; Keller et al., 2010; Petosa et 214 768 1991; fax: +1 214 768 2164. al., 2010; Ottofuelling et al., 2011). In general, nanoparticle agglom- E-mail addresses: [email protected] (L.A. Seders Dietrich), [email protected] eration increases with increasing ionic strength, and agglomeration (M. Sahu), [email protected] (P. Biswas), [email protected] (J.B. Fein). 1 Present address: Advanced Energy Technology Initiative, Prairie Research Institute, also increases as the suspension pH approaches the zero point of University of Illinois at Urbana—Champaign, Champaign, IL 61820, USA. charge (pHzpc) of the nanoparticles (e.g., French et al., 2009; Jiang 0009-2541/$ – see front matter © 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.chemgeo.2012.09.043 L.A. Seders Dietrich et al. / Chemical Geology 332–333 (2012) 148–156 149 et al., 2009). Agglomerate size also increases as the pH approaches Briefly, the nanoparticle sizes reported here were based on the equiva- the pHzpc (Dunphy Guzman et al., 2006; Fatisson et al., 2009). The lent diameter of the particles as determined by their measured surface presence of other dissolved components, such as cations, organic area. The same particles were also measured by microscopic methods matter, or surfactants, can also affect the agglomeration behavior of by counting more than 100 particles from representative images. Infor- TiO2 nanoparticles (Tkachenko et al., 2006; Domingos et al., 2009; mation on the average particle size and standard deviation is given in French et al., 2009; Joo et al., 2009; Keller et al., 2010; Ottofuelling more detail in Jiang et al. (2008). The nanoparticles were observed to et al., 2011). be spherical, and each size fraction contained a range of particle sizes Nanoparticle agglomeration behavior can affect or be affected by in- (Jiang et al., 2007, 2008; Sahu et al., 2011). The average diameters teractions with geosorbents (Dunphy Guzman et al., 2006; Choy et al., (dry) of the three nanoparticle size fractions used in these experiments 2008; Fang et al., 2009; Fatisson et al., 2009; Joo et al., 2009; Solovitch were 16 nm, 26 nm, and 50 nm. The hydrodynamic diameter of the et al., 2010), significantly influencing particle transport. Dunphy particles (i.e., agglomerate size) is known to change with ionic strength Guzman et al. (2006) found that larger agglomerates had higher inter- and pH (Jiang et al., 2009; Sahu et al., 2011), and agglomeration was action energies, which led to an increase in nanoparticle deposition; expected under our experimental conditions. The crystallinity and however, TiO2 nanoparticles and their agglomerates were still found phase of the material were determined using X-ray diffractometry to be highly mobile under most conditions. Fatisson et al. (2009) (XRD) with a Rigaku D-MAX/A9 diffractometer and Cu Kα radiation found that the deposition rates of TiO2 nanoparticles onto silica differed (λ=1.5418 Å). The crystalline phase of the material was anatase as de- depending upon changes in pH and ionic strength due to the effect of termined from the XRD pattern. The resulting nanoparticles were in these parameters on particle agglomeration. Nanoparticle agglomera- powder (dry) form and were used without washing. Specific surface tion and deposition were also observed by Fang et al. (2009) to depend areas determined previously for TiO2 nanoparticles of similar size and upon the characteristics of the soil with which the nanoparticles were in manufactured using the same process were 95.8, 61.5, and 31.5 m2/g contact. As is true of most particles, high ionic strength, pH, and zeta po- for the 16, 26, and 50 nm particles, respectively (Jiang et al., 2007, tential affected TiO2 settling, while increasing the dissolved organic car- 2008, 2009). The isoelectric points of nanoparticles manufactured bon concentration and clay content helped to stabilize the nanoparticles using the same procedure described above were shown previously to in suspension. In some cases, the formation of large agglomerates with- decrease with increasing nanoparticle size from pH 5.8 at 16 nm to in soil columns completely prevented their passage (Fang et al., 2009). pH 5.2 at 26 nm to pH 5.0 at 53 nm (Suttiponparnit et al., 2010). Using sand columns, Choy et al. (2008) found almost complete reten- tion of TiO2 nanoparticles, although the roles of straining and adhesion 2.2. Geosorbents could not be differentiated. Joo et al. (2009) observed similar retention of TiO2 nanoparticles in silica columns, but in the presence of an The geosorbents used in these experiments were amorphous sil- adsorbed polymer, nanoparticle transport was enhanced. Thus, TiO2 ica gel (30–60 mesh) purchased from Sigma Aldrich (St. Louis, MO), nanoparticles remain disagglomerated and mobile in certain soils and as well as this same amorphous silica onto which an Fe(III) oxide under certain aqueous conditions, but they agglomerate and become coating was applied following the procedure of Ams et al. (2004) immobile due to straining and/or adhesion in others. This change in mo- (described in more detail in the Supplementary materials). The silica bility as a function of agglomeration state is true of most particles over a grains to which the Fe(III) oxide coating was applied will hereafter range of compositions and sizes.
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