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Chemosphere 71 (2008) 2091–2097

Particle-facilitated lead and arsenic transport in abandoned mine sites soil influenced by simulated acid rain
Shaoping Hu, Xincai Chen *, Jiyan Shi, Yingxu Chen, Qi Lin
Department of Environmental Engineering, Zhejiang University, Hangzhou 310029, PR China Received 19 September 2007; received in revised form 13 January 2008; accepted 15 January 2008 Available online 10 March 2008

Abstract The role of acid rain in affecting Pb and As transport from mine tailings was investigated by pumping simulated acid rain at a infiltration rate of 10.2 cm/h through soil columns. Simulated acid rain with pH of 3.0, 4.5 and 5.6 were used as leaching solutions. Results showed that 86.9–95.9% of Pb and 90–91.8% of As eluted from the columns were adsorbed by particles in the leachates. Scanning electron microscopy (SEM) analysis showed that particles released from the columns were mainly composed of flocculated aggregates and plate or rod shaped discrete grains. Transmission electron microscopy (TEM) coupled with energy dispersive X-ray analysis (EDX) showed that these particles were predominantly silicate minerals. Results from our experiments demonstrated that when rapid infiltration conditions or a rainstorm exist, particle-facilitated transport of contaminants is likely to the dominant metal transport pathway influenced by acid rain. Ó 2008 Elsevier Ltd. All rights reserved.
Keywords: Metal; Mine; Column; Contaminant; Leachate

1. Introduction To make an accurate assessment of the ecological risk of contaminants in soil, it is necessary to be able to quantitatively estimate the mobility of contaminants. However, attempts to describe and predict contaminant transport cannot succeed if major pathways and mechanisms for transport are not defined (McCarthy and Zachara, 1989). Most predictions of contaminant transport have been based on a two-phase system in which contaminants partition between the immobile solid constituents and the mobile aqueous phase (McCarthy and Zachara, 1989; Puls and Powell, 1992; Grolimund et al., 1996). It is generally assumed that metals are adsorbed by the soil solid phase with low mobility in soil. Some particles in the soil solid phase, however, also may be mobile in soil, and these particles are relatively reactive with respect to sorption of chemical species due to their large specific surface area
Corresponding author. Tel.: +86 571 86971424; fax: +86 571 86971898. E-mail address: (C. Xincai). 0045-6535/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved. doi:10.1016/j.chemosphere.2008.01.024

and high number of functional surface groups (Lagdsmand et al., 1999). Once mobilized, these particles may bind contaminants and enhance contaminant transport in soil (McCarthy and Zachara, 1989; Grolimund et al., 1996; Ryan and Elimelech, 1996; Kersting et al., 1999; Flury et al., 2002; Lowry et al., 2004). Acid deposition is a global environmental problem in terrestrial and aquatic ecosystem, resulting in a series of chemical reactions that enhance toxic metal mobilization in soil ecosystems. The link between metal mobilization and acidifying soil processes have been explored in several papers (Sverdrup et al., 1994; Wilson and Bell, 1996; Mannings et al., 1996; Gong and Donahoe, 1997; Bini and Bresolin, 1998; Walna et al., 1998; Larssen et al., 2000). However, previous studies mostly emphasized the impact of acid rain on metal solubility, and concluded that the pH of acid rain was the main factor altering the mobility and speciation of metals in soil. At this time, there are few data on the possible role of particle-facilitated transport of heavy metals in contaminated soils as affected by acid rain. It is reasonable to expect that soil pH changes could alter particle-facilitated metal transport, but laboratory

All above analyses were conducted in triplicate. 1994). 4. The resulting slurries were wet sieved in deionized water using 2 mm. organic matter content and cation exchange capacity (CEC) were determined according to the methods described by Lu (1999). respectively. and 8 lmol lÀ1. The clay fraction (<2 lm) was isolated by sedimentation of the <20 lm fraction (Isaure et al. ground and sieved to pass through a 2 mm plastic mesh for further use. The columns were oriented vertically and slowly saturated from the bottom with 73. 21. 3 ml of 6 N HCl was added to the residue for final dissolution (Isaure et al. 2. The tailings from the mining operation were surface-deposited over the past centuries until 1950. The aim of the present study is to evaluate the mobility of lead and arsenic in a mine tailings polluted soil influenced by simulated acid rain over a range of pH. a relatively lower pH may inhibit release of particles in soils (Ryan and Gschwend.6. The leachates were collected with 100 ml glass collectors. pumped by HPLC pump to percolate through the packed soil columns. and porosity about 70%. 2..2. Mg2+. SO42À. Undispersed samples were analyzed after shaking with water for 10 min. silt and clay were 64%. 1996). and 16.5%. 2002). A previous survey indicated that the total concentration of lead and arsenic in the surface soil exceeds 10 000 mg kgÀ1 and 5000 mg kgÀ1 respectively..0 cm3 minÀ1) and stabilized for 24 h. Chemical analyses Bulk soil samples and fractions were further ground to pass through a 160 lm plastic mesh. The feed solutions were simulated acid rain with pH 3. 4. 2. 5.12°/min (Isaure et al.6 cm3.6. 44.5. 200 lm. Ca2+.5 to 5. Experiments were conducted in triplicate at each pH. 21. We selected sites containing relatively high lead and arsenic to sample soils for the experiments.. In order to reliably explain the influence of pH on metal migration. Airdried soil aggregates (<2 mm) were tamped into the columns to a uniform bulk density of %1.3.1. and redissolved with HCl.6 g soil aggregates used for each column. After evaporation of the solution. The suspensions were ultrasonically dispersed by an ultrasonic generator (Branson W-185C) for 30 min. Conversely. and 20 lm mesh size. Soil pH. 2002). X-ray diffraction patterns were recorded on powders over 4°–90° 2h at a scan speed of 0. respectively. The mean regional rainfall is 1800 mm/year with peak intensities exceeding 110 mm/h due to the influence of summer typhoons. 2. with approximately 122.5 g of solid in a Teflon bomb and heating to 200 °C to completely digest. 24. it is necessary to separately measure the ‘‘particulate” and ‘‘dissolved” fraction of metals in soil leachates.. the morphology and chemical composition of eluted particles were investigated.3% of claysized particles exist as aggregates. the pH of rainfall varied from 3. and 5.5. Leachate analysis A 1 ml aliquot of leachate was digested by adding HF and HNO3 to a Teflon bombs with heating to 200 °C to completely digest. The percentages of sand. Synthetic acid rain of pH 3. 500 lm. The length of the soil columns in glass tubes were approximately 25 cm with a typical pore volume (PV) of 73. 2.2 cm/h (Grolimund et al. The degree of soil aggregation is represented as the ratio of the proportions of clay-sized particles (<2 lm) in dispersed and undispersed soil (McDowell and Sharply.2. In addition. more than 10 topsoil (2– 20 cm) samples were collected.5%. diluted to 10 ml with DI water and then analyzed by ICP-AES. NH4+. Simulated rain preparation At the sampling site. Simulated acid rain was designed according to the main ion composition and pH of local rain water. / Chemosphere 71 (2008) 2091–2097 experiments have demonstrated that release of mobile colloids in most soils are favored by high pH (Swartz and Gschwend.6 was prepared from a stock H2SO4–HNO3 solution mixture(4:1 v/v). 96. Each column was flushed with a total of 50 PV incoming solution. the acid was evaporated to almost dryness.0 g cmÀ3.0. 2002).5 mA). 1994). 1998. 2002). The particle-adsorbed and dissolved fractions of metals were quantitatively determined in the soil column leachates. Bulk soil mineral identification was performed using a Siemens D501 powder diffractometer with Co Ka radiation (40 kV and 37. and 5. Materials and methods 2. Soil analysis Particle size analysis was conducted using 50 g air-dried in 2000 ml beakers and 300 ml deionized water added to the beaker. This measurement represents the total (dissolved and particulate) elemental . Soil collection Soils were collected from an old mining site named Silver Mountain located in the middle of Zhejiang province in south-east China. Bunn et al. 2. digested by adding 9 ml of HF and 1 ml of HNO3 to 0.5. ClÀ. 50 lm.2092 S.6 cm3 (1 PV) deionized water (1. We used a flow rate of 50 ± 5 cm3/h. 33. Na+. Elemental concentrations were measured by inductively coupled plasma atomic emission spectrometer (ICP-AES). composited by mixing together and air-dried. which correspond to field infiltration velocities of 10.0. results showed that 41. The tested site is a paddy soil with loamy texture.The concentration of K+. 2003). A nylon screen (120 lm) and oring (25 mm diameter) was used to retain the soil in the columns (Ryan and Gschwend. NO3À and FÀ were 8. Hu et al. 19.4. Laboratory column experiment Column experiments were performed in 30 cm long glass tubes columns with an interior diameter of 25 mm..

that is. muscovite. the concentrations of Fe. / Chemosphere 71 (2008) 2091–2097 2093 concentration in the column effluents. with particulate Pb accounting for 86. cation exchange capacity. release of Pb and As (sum of the dissolved and particulate) reached a steady-state with the concentrations generally stabilizing at 1. Percentage of total As.7 ± 1.81 ± 0.27 mg lÀ1 in the initial effluent to 0.0 ± 0. There was a significant influence of pH on dissolved Pb in column outflows(r = 0.9–95. Hu et al. 1996). mean ± standard deviation.04 mg lÀ1 to 0..0 ± 1.0 ± 4.2 15 806 ± 847 9.9% of total released Pb.S. There was no significant difference in the amount of total released Pb and As from columns at different pH.3. Table 2 Weight percentage of grain-sized fractions and relative Pb and As concentration as a function of soil particle sizea Particle size (lm) Weight percentage (%) As <2 16.9 4 977 ± 483 3. Percentage of total Pb. However. Release of Fe. 1a and b). concentration of Pb in bulk soil. These results reveal that the mobility of Pb and As are mainly controlled by particulate species.2 5 322 ± 591 10.2 0.2 500–1000 10.1 ± 2. The relative Pb and As concentration as a Table 1 Selected characteristics of contaminated soil Parameters pH Valuea a b c d e function of soil particle size is given in Table 2. Another 12 ml aliquot of effluent sample was ultracentrifugated at 2 Â 105 g for 2 h (Grolimund et al.0 ± 3. and the average values of measured concentrations were used. Pb.7 ± 0.02 mg lÀ1 after 2 PV and gradually reached a baseline level around 0.10 mg lÀ1 for As (Fig.01).3 ± 1.6 19 252 ± 982 19. concentration of As in bulk soil. and montmorillonite. As. Si and Al from soil columns In order to identify the particle composition in column effluents.1 10 ± 0.1–91.8 18 397 ± 816 21.2 ± 1.1.3 ± 1.3 ± 1.7. particulate facilitated transport is the dominant transport pathway for Pb and As under the elevated flow conditions used in this study.859. 2.4 2–20 19. mean ± standard deviation.8 16 916 ± 532 5328 ± 409 In triplicate.5 Pb a b c In triplicate. XRD analysis showed that the soil sample mainly contains quartz.5 ± 1. Table 3 summarizes the cumulative amount of each species of Pb and As in column effluent after 50 PV elution. SEM. 3. there was no significant difference in dissolved As concentrations in column effluent at different pH. coated by Au and characterized by SEM (KYKY-1000B).9 ± 0.4 200–500 13. 1c and d. At pH 3.3 ± 1.2. the concentration of dissolved Pb in effluents gradually decreased from 0. TEM-EDX analysis The particles present in the leachates.1 ± 1. Dissolved Pb and As released from packed columns as a function of infiltration volume are shown in Fig. There was no significant difference between Pb and As distributions among soil size fractions. and 45% of Pb and 40% of As were found in relatively smaller sized fractions (<20 lm). Al and Si in leachates OMb (%) CECc Pbd À1 (cmol kg ) (mg kgÀ1) Ase (mg kgÀ1) 5.5 ± 1. The other was re-suspended in ethanol.8 ± 0. The supernatant. The particulate As and Pb were calculated from the difference between total and dissolved concentration. The EDX investigation was carried out at an 80 nm spot at 60 keV. Bulk properties of contaminated soil Selected characteristics of contaminated soil are shown in Table 1. One was sprinkled onto 2 cm2 plates.4 4 297 ± 378 12.4 1000–2000 3.3 Concentration (mg kgÀ1) Percentageb (%) Concentration (mg kgÀ1) Percentagec (%) 7 654 ± 582 24.3 17 477 ± 864 13. organic matter content.8 50–200 21. clinochlore. Results 3. and particulate As accounting for 90. while dissolved As rapidly decreased from 0. OM. Each analysis was conducted in triplicate.0. with a drop of this suspension evaporated onto carbon-coated copper and analyzed by TEM (Philips CM120) equipped with an EDX system (PHOENIX).5 ± 2.10 mg lÀ1 at the end of the experiments. .2 11 962 ± 613 11. were separated by ultracentrifugation. containing only the dissolved As and Pb species (<20 nm). Release of Pb and As from soil columns After eluting approximately 30 PV simulated acid rain. p < 0.6 4 457 ± 247 11. Total concentrations of released As and Pb were always well correlated in column outflows at different pH levels.10 mg lÀ1 for Pb and 0. 3.5 15 970 ± 698 20. 3. CEC.8% of the total released As.2 ± 3.01 mg lÀ1.7 18 833 ± 885 3.5 ± 1. freeze-dried and divided into two subsamples.2 4 106 ± 265 16. was carefully pipetted into a pre-cleaned plastic bottle and analyzed by ICP-AES.1 5 756 ± 601 21.6 ± 1.0 ± 3.7 20–50 15.

4.9 ± 6.1 Totalc (mg kgÀ1) 4.0 pH4. Morphological identification of mobile particles Typical features of particles released from columns by acid rain leaching are shown in Fig.025 0.0 pH4.6 PV PV c Dissovled Pb mg l -1 0.1 ± 2. dissolved Fe and Al in column effluent significantly decreased (r = 0. could signifi- . 4.5 pH5. Total Pb released from soil samples in columns.015 0. with the larger difference between total released and dissolved Fe and Al indicating that more particulate Fe and Al were released from soil columns at pH 5.5 0.31 Particulate (%) 90.0 0 10 20 30 40 50 pH3. 1996).1 ± 5.2094 S.3 0. Based on the micrographs.9 In triplicate.01).1 ± 5. and physical conditions such as pore structure.9 ± 6.5 pH5. Total As released from soil samples in columns. and influent pH had no significant influence on particulate Si in the column effluent.0 38.5 2.6.1 0.6 ± 1.0 3.4 8.9 95.6. / Chemosphere 71 (2008) 2091–2097 a Total Pb mg l-1 4. 1. Ca.0 pH4.6 d 0.010 0. (b) total As.4.7 91. Al.30 0.6.1 ± 1.5 3.5.09 0. hydrodynamic forces and size of particles.4 0. Si. mean ± standard deviation.7 ± 4.1 Dissolved (%) 9.27 0. such as pH and ionic strength.0.6. and (d) dissolved As from columns as a function of elution volume at pH 3.1 ± 0.15 0. Release of (a) total Pb. Particulate Si was high in leachates at all pH. In agreement with this. Chemical conditions. concentrations of dissolved Fe and Al were close to total Fe and Al in column outflows. 2). 3e and f).035 0. At pH 3. Acid pH had no significant influence on total concentration of Fe and Al in column effluent (p > 0. indicating that Fe and Al mainly existed as dissolved species in soil columns at more acid pH. 3a and b.0 2.7 35.4 90.045 0.6 a b c As Particulate (%) 86.5 pH 5.5 Dissolved (%) 13.24 0.21 0. Some flat or rod shaped discrete grains in flocculated aggregates were also observed by SEM.8 0.9 ± 0.9 ± 0. (c) dissolved Pb. TEM–EDX analysis indicated that the main elemental components of aggregates are O.020 0.55 4.8 34.06 0.0 pH 4.2 ± 6.62 4. p < 0.0 0 10 20 30 40 50 pH3.5 pH5.5 pH5.7 0.2 5.005 0.4 ± 4.6 9.0 to 5. Table 3 The proportion of each species of Pb and As in columns effluents after 50 PV elution by simulated acid raina Pb Totalb (mg kgÀ1) pH 3.2 0.3 4. K. Discussion It is well known that metallic elements become more soluble under acidic conditions (Wilson and Bell.1 94. particles ranged in size from the limits of SEM resolution (about 50 nm) to about 20 lm at all pH values in these experiments.0.12 0.3 ± 1. Si.3 ± 3.000 pH3. Unlike the above-mentioned elements which exist in aggregates. 3c and d). Mg and Fe (Fig. When the influent pH increased from 3.5 1.05).0 0.6 0. 3.040 0.6 b Total As mg l-1 0. more Pb.0 pH4.0 and 5. and 5.030 0. As.and Al-oxide (oxyhydroxide).0 1. Fe and a part of the Al may come from Fe.03 0.6 10 20 30 40 50 0 10 20 30 40 50 PV PV Fig. as a function of infiltration volume were investigated (Fig. Pb and S were localized in some discrete particles (Fig.8 ± 6.2 ± 1. Hu et al. Al and Fe were dissolved in columns at more acid pH induced by simulated rain (Table 3).18 0. At pH 3.5 0.00 0 Dissolved As mg l-1 pH3.9 ± 2.866.

Sen and Khilar (2006) stated that hydrodynamically induced release of fine fractions is found to be of more common occurrence in loose soil embankments and in packed beds. In present experiment. 2006).0).5. p < 0. 2004). Hu et al. (1997) determined that amorphous ferric oxyhydroxide (representing only 5% of the total iron) can play a significant role in the binding of clay colloids to aquifer grains.6. They pointed out the two major reasons for hydrodynamically induced release: (a) the flow velocity encountered is high. p < 0. can be a source of mobile particles.0.. 2. / Chemosphere 71 (2008) 2091–2097 2095 a Concentration (mg l-1) 10 9 8 7 6 5 4 3 2 1 0 Concentration (mg l-1) TAl TFe TSi DAl DSi DFe b 10 8 6 4 2 0 0 10 20 30 40 TAl DAl TSi DSi TFe DFe 0 10 20 30 40 50 50 PV PV 10 8 6 4 2 0 0 10 20 30 40 50 TAl DAl TSi DSi TFe DFe c Concentration (mg l-1) PV Fig. and re-adsorbed by layer silicate minerals. Fe or Al oxide could partially dissolve to increase Pb and As release in soil at more acid .2 cm/h is a very high infiltration rate. p < 0. Results showed that particulate Si in leachate is well correlated with total released Pb (r = 0. these larger sized particles may be mobilized by hydrodynamically induced release. namely the hydrodynamically induced release. may act as a vector of contaminant transport at acid pH. which normally have pHpzc < 4. total released Pb was strongly correlated to Fe (r = 0.01). p < 0. as illustrated by the prevalence of particulate Si in the column leachates in the present work. Dong et al. 10. Results from SEM observation showed some mobile particles are larger than 20 lm.01). 2000. muscovite and clinochlore.885. indicating that Pb was associated with Fe or Al oxides in leachate. In the present experiments.871. Results from this work showed that particulate Pb and As were also prevalent in effluents collected from acid rain leaching.. cantly influence particle release in soil (Sen and Khilar. 5. 1997. 1996). These phenomena indicate that the dissolution of an Fe/Al complex may participate in the process of Pb and As release. and (c) 5. Another factor that should be taken into account is the flow rate.0. and (b) the particles are usually of large size and thereby experience a large drag force. Conclusion Results from the present experiments demonstrated that when rapid infiltration conditions or a rainstorm exist.01) and As (r = 0. 1996. Concentration of total released Al/Si/Fe(TAl/TSi/TFe) and dissolved Al/Si/Fe(DAl/DSi/DFe) in column effluents as a function of elution volume at pH (a) 3. The dominant minerals in the bulk soil samples such as montmorillonite.01). (b) Pb and As are released due to a dissolution process. Lee et al. at less acid pH (5. thus relatively large particles were possibly washed out from soil columns.S. At lower pH (3.887. (b) 4. There are two possible mechanisms explaining Pb and As association with Si: (a) Pb and As are bound to layer silicate minerals directly released from soil flushed by acid rain.6). even at pH 3. total released Pb was strongly correlated to dissolved Fe (r = 0.. Silicate minerals could be a carrier of Pb and As to facilitate transport in soil.01) and Al (r = 0. Swartz et al.967. p < 0. particle-facilitated transport of Pb and As is likely to represent the dominant transport pathway in soil influenced by acid rain. Hartley et al.974. Layer silicate minerals. Numerous published experimental data along with the theoretical evidence suggest that Pb and Fe/Al are associated in soils (Routh and Ikramuddin. Studies have shown that point of zero charge (pzc) of colloids is one of the key factors that control colloid release in variably charged soil (Ryan and Elimelech.

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