Enhancement of Arsenic Adsorption during Mineral Transformation

Article pubs.acs.org/est

Enhancement of Arsenic Adsorption during Mineral Transformation from Siderite to Goethite: Mechanism and Application Huaming Guo,*,†,‡ Yan Ren,‡ Qiong Liu,‡ Kai Zhao,†,‡ and Yuan Li†,‡ †

State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Beijing 100083, P.R. China School of Water Resources and Environment, China University of Geosciences, Beijing 100083, P.R. China

‡

S Supporting Information *

ABSTRACT: Synthesized siderite was used to remove As(III) and As(V) from water solutions under anoxic conditions and oxic conditions. Results showed that As adsorption on synthetic siderite under anoxic conditions was around 10 mg/g calculated with Langmuir isotherm. However, the calculated As adsorption on synthetic siderite under oxic conditions ranged between 115 and 121 mg/g, which was around 11 times higher than that under anoxic conditions. It was found that 75% siderite was transformed into goethite during oxic adsorption. However, synthetic goethite had lower As adsorption capacity than siderite under oxic conditions, although its adsorption capacity was a little higher than siderite under anoxic conditions. It suggested that the coexistence of goethite and siderite bimineral during mineral transformation probably contributed to the robust adsorption capacity of siderite under oxic conditions. Results of extended X-ray absorption fine structure (EXAF) spectroscopy indicated both As(III) and As(V) formed inner-sphere complexes on the surface of As-treated solid regardless of substrates, including the bidentate binuclear corner-sharing (2C) complexes and the monodentate mononuclear corner-sharing (1V) complexes. Monodenate (1V) and bidentate (2C) complexes would be related to high As adsorption capacity of siderite under oxic conditions. It showed that more Fe atoms were coordinated with As atom in the monodentate complexes and the bidentate complexes of As(V)/As(III)treated siderite under oxic conditions, in comparison with As(V)/As(III)-treated siderite under anoxic conditions and As(V)/ As(III)-treated goethite. Calcinations of natural siderite resulting in the coexistence of goethite and siderite greatly increased As adsorption on the solid, which confirmed that the coexistence of bimineral during mineral transformation from siderite to goethite greatly enhanced As adsorption capacity of siderite adsorbent. The observation can be applied for modification of natural siderite for As removal from high As waters.

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INTRODUCTION High As groundwater has been regarded as a serious worldwide environmental issue.1 Hundreds of millions of people are at risk from drinking As-contaminated groundwater in the world,2 which has been found in many countries. Arsenic in drinking groundwater could cause skin cancer and internal cancers, particularly of the lung and urinary tract.3 Consequently, the World Health Organization has set a provisional guideline limit of 10 μg/L for As in drinking water, which has been subsequently adopted by the European Union, the United States, and China.3,4 It is obligated to remove As from potential drinking water with As concentrations greater than 10 μg/L. In addition to natural processes, anthropogenic activities resulted in As contamination in water by means of mining, wood preservation, arsenic-containing pesticide utilization, and glass manufacturing, which usually produced wastewater with high As concentrations. Arsenic concentrations in mining drainage ranged between 50 to 850,000 μg/L.1 Arsenic removal from both drinking groundwater and wastewater has received much concern. © 2012 American Chemical Society

Iron-containing substances have been widely studied to remove As from aqueous solution due to their high specific surface area, positive surface charge at neutral pH, and sufficient adsorption sites, including Mn-substituted Fe oxyhydroxide,5 granular ferric hydroxide,6 ferrihydrite,7 goethite,8 zerovalent iron,9 Ce(IV)-doped Fe oxide,10 natural hematite and natural siderite,11 green rust,12,13 and magnetite.14 Among these materials, Fe(II, III) systems have received much concern due to the occurrence of electron transfer, adsorption, and coprecipitation during the interaction between adsorbents and As species.15−18 Rapid oxidation of As(III) to As (V) was observed in Fe(II)−Fe(III) systems under anoxic conditions and Fe(II)−O2 systems under oxic conditions.15,17,28,40,41 Reactive Fe(III) species, forming as an intermediate Fe(III) phase in Fe(II)-goethite system, were proposed to rapidly Received: Revised: Accepted: Published: 1009

August 30, 2012 December 13, 2012 December 19, 2012 December 19, 2012 dx.doi.org/10.1021/es303503m | Environ. Sci. Technol. 2013, 47, 1009−1016

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through a 0.22 μm filter, and finally analyzed for dissolved total As and As species. Natural siderite and modified natural siderite were used to evaluate enhancement of As adsorption on bimineral adsorbent during partial mineral transformation from siderite to goethite. The natural siderite (with grain size of 0.5−1.0 mm) was modified by calcination at 300 °C for about 4 h. After modification, siderite content decreased from 69.2% to 40.4%, while goethite increased from 0.89) were obtained (Figure 4). Adsorption capacities for As(III) and As(V) calculated from Langmuir isotherm fitting were 12.2 and 11.2 mg/g, respectively (Table 1). The values were comparable to those reported by Ladeira and Ciminelli (12.5 mg/g for As(V))24 and a little higher than those reported by Manning et al. (6.8 mg/g and 4.5 mg/g for As(III) and As(V), respectively).25 These adsorption values were a little higher than those on pure

Figure 4. Adsorption of As(V) and As(III) on synthesized goethite under oxic conditions (dosage = 2 g/L; initial As concentration = 2.0− 600 mg/L; contact time = 6 h; at 25 °C).

siderite but much lower than those on synthetic siderite under oxic conditions in this study. It was inferred that goethite itself would not be expected to contribute to robust adsorption capacity for inorganic As species on siderite under oxic conditions. Although the specific surface area of goethite (24.2 m2/g) is lower than those of siderite under oxic conditions (95.8−110 m2/g), the values of its surface coverage for As(III)/As(V) (5.2−7.5 μmol/m2) are lower than those on As(III)/As(V)-treated siderite under oxic conditions (12.2− 13.2 μmol/m2) (Table 2). It suggested that the surface area may not be the major factor enhancing As adsorption, although the role of goethite crystallinity cannot be ruled out in As adsorption. Therefore, enhancement of As adsorption during mineral transformation would be expected to relate to the presence of siderite-goethite bimineral systems, promoting redox processes, adsorption, and complexes between solids and As species. 1012

dx.doi.org/10.1021/es303503m | Environ. Sci. Technol. 2013, 47, 1009−1016


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Table 2. EXAFS Fit Parametersa for As(V)/As(III)-Treated Siderite and Goethite samples As(V) siderite (oxic)

As(V) siderite (anoxic)

As(V) goethite (oxic)

As(III) siderite (oxic)

As(III) siderite (anoxic)

As(III) goethite (oxic)

interatomic shellb

R (Ǻ ) (±0.03)

N (±0.5)

σ2 (Ǻ 2) (±0.0001)

Γc (μmol/m2)

As−O MS As−Fe1 As−Fe2 As−O MS As−Fe1 As−Fe2 As−O MS As−Fe1 As−Fe2 As−O MS As−Fe1 As−Fe2 As−O MS As−Fe1 As−Fe2 As−O MS As−Fe1 As−Fe2

1.69 3.11 3.35 3.50 1.69 3.11 3.34 3.45 1.69 3.11 3.34 3.45 1.71 3.13 3.35 3.52 1.78 3.12 3.35 3.46 1.76 3.15 3.33 3.45

3.8 4.6 2.5 1.8 4.0 6.9 2.0 1.0 4.0 3.0 2.1 1.1 3.5 4.4 3.2 2.2 2.8 3.4 1.8 0.9 2.9 6.0 1.7 0.9

0.0006 0.0049 0.0045 0.0034 0.0033 0.0063 0.0058 0.0013 0.0028 0.0014 0.0020 0.0053 0.0026 0.0066 0.0027 0.0058 0.0033 0.0026 0.0014 0.0024 0.0032 0.0026 0.0012 0.0017

13.2

predominated in the As(III)-treated goethite sample performed under oxic conditions (Figure 5a), which meant that oxidation of As(III) had been limited. This observation was also reported by Manning et al.,25 Farquhar et al.,26 and Ona-Nguema et al.,27 who found no detectable As(V) in As(III)-treated goethite under oxic/anoxic conditions. However, As(III)-treated siderite under oxic conditions gave clear evidence of partial As(III) oxidation to form a mixed As(III)/As(V) speciation in the solid (Figure 5a). There was no evidence found for As(III) oxidation by the X-ray beam. In oxic conditions, As(III) was expected to be readily oxidized by reactive intermediates formed during the oxidation of Fe(II) in siderite batches by O2.15,28 Ona-Nguema et al. also proposed that strongly oxidizing radical species produced by the oxidation of Fe(II) by dissolved O2 contributed to rapid oxidation of As(III) to As(V).40 Such reactive radical species can be produced during Fenton-like processes.40,41 The rapid As(III) oxidation was also found in the Fe(II)−Fe(III) system15,28 and iron oxides and oxyhydroxides synthesized from Fe(II).29 In the system of Fe0−As(III) under oxic conditions, As(III) oxidation was observed during the Fe0 corrosion reactions or after, partially due to the coexistence of magnetite and maghemite.30 As(III) oxidation along with the presence of Fe(II)−Fe(III) bimineral and O2 suggests that Fenton-type reactions occur, that generally require Fe(II) and O2 in aqueous solutions. After 6 h reaction, Fe(III) species accounted for around 80% of total Fe in the solid calculated from Fe EXANES analyses (data not shown). XRD results also showed Fe(II) oxidation with production of goethite (75%). The oxidation processes were consistent with the high adsorption for As in As(III)-treated siderite under oxic conditions, suggesting that As(III) oxidation and complexes between Fe(II)−Fe(III) minerals and As species greatly improved As adsorption. Arsenic(V)-treated samples showed no redox transformations of adsorbed As(V) (Figure 5b). Although no redox transformations of adsorbed As(V) were observed in As(V)treated siderite, there was a big difference in As(V) adsorption on siderite between anoxic conditions and oxic conditions. The greater adsorption for As(V) under oxic conditions than that under anoxic conditions would be related to Fe(II) oxidation and the presence of siderite-goethite bimineral (Figures 3b and 3d). Besides, the higher adsorption for As(V) than As(III) with initial As concentration ≤100 mg/L possibly implied the predominant role of goethite of bimineral in As removal. With initial As concentration >200 mg/L, the key controlling factor for the higher adsorption for As(III) than As(V) may be related to As(III) oxidation. The experimental radial structure functions (RSF) obtained from Fourier transformed EXAFS data are shown in Figures 6 and 7. The fits of the theoretical EXAFS expression to the experimental data are also shown (dotted lines, Figures 6 and 7), and the fitted parameters are given in Table 2. The first coordination shell surrounding As in the As(V)-treated samples was well fit by 3.8−4.0 oxygen atoms at an As−O distance of 1.69 Å (Figure 6 and Table 2), corresponding closely to the expected As(V)−O distance (i.e., 1.69 Å in the AsO 4 tetrahedron molecule). This distance was consistent with previously EXAFS studies for As(V) on goethite, siderite and magnetite,23 lepidocrocite and maghemite.30 The predominant feature of As(III)-treated siderite under oxic conditions is the first shell of 3.5 ± 0.5 oxygen atoms at an As−O distance of 1.71 ± 0.03 Å (Figure 7 and Table 2),

1.8

5.2

12.2

1.0

7.5

R (Å), interatomic distances; N, number of neighbors; σ2 (Ǻ 2), Debye−Waller parameter. bMS, As−O−O−As multiple scattering paths. cΓ, the values of surface coverage were calculated from the adsorbed amounts of As(V)/As(III) in μmol/m2. Since synthesized siderite may be partially oxidized during BET surface area measurement, its specific surface area would be a little higher than actual one. a

Mechanisms. The XANES spectra of As(III)-treated siderite under anoxic conditions and goethite samples under oxic conditions were collected to test for possible As(III) oxidation to As(V) (Figure 5a). As(III)-treated siderite showed energy position indicative of As(III), suggesting that oxidation to As(V) on the surface had not occurred. It was consistent with results of As species in solutions of the batches. Jönsson and Sherman also found no As(III) oxidation in As(III)-treated siderite under anoxic conditions.23 Similarly, As(III) was

Figure 5. Arsenic K-edge XANES spectra for As(III)-treated materials (a) and As(V)-treated materials (b). 1013



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As path. For As(V)-treated samples, an As−Fe distance of 3.34−3.35 Å dominated the second-neighbor contribution, regardless of substrate (Table 2). This was in good agreement with the distances for As(V) on goethite and lepidocrocite,30 As(V) on maghemites,31 As(V) on siderite (anoxic),23 and As(V) on green rust (anoxic) (S1 in the Supporting Information).13 The As−Fe distance of 3.3−3.4 Å indicated the presence of bidentate binuclear corner-sharing (2C) complexes.30,32−34 An additional long As−Fe distance of 3.45−3.50 Å contributed to the second-neighbor signal in those samples (Table 2), which was consistent with the distances for As(V) on lepidocrocite and goethite30 and As(V) on green rust (anoxic).13 It indicated that the monodentate mononuclear corner-sharing (1V) complexes were also formed on the surface of the samples.13,30,31,34 In the present study under high surface coverage conditions (Γ = 1.8−13.2 μmol/ m2), the 1V complexes were found to coexist with the 2C complexes, which suggested that the existence of 1V complexes was favorable under high surface coverage conditions.27,35,36 For As(III)-treated samples, the As atom was coordinated by 1.7−3.2 Fe atoms with RAs−Fe = 3.33−3.35 Å and 0.9−2.2 Fe atoms at RAs−Fe = 3.45−3.52 Å, respectively, regardless of substrate (Table 2). The short distance of As−Fe (3.33−3.35 Å) was consistent with the distances for As(III) on goethite (anoxic) and lepidocrocite (anoxic),27 As(III) on goethite (oxic),25 As(III) on goethite (oxic),30 and As(III) on goethite (anoxic) (S1 in the Supporting Information),23 which was considered to be the bidentate binuclear corner-sharing (2C) complexes.27,13 Besides, the As−Fe distance of 3.45−3.52 Å was due to the monodentate mononuclear corner-sharing (1V) complexes, for which the average distance was 3.5 ± 0.1 Å in ludlockite.27,37 The distance was in good agreement with the As−Fe distances for As(III) on goethite (anoxic) and lepidocrocite (anoxic)27 and As(III) on maghemite (anoxic) (S1 in the Supporting Information).31 Both the bidentate binuclear corner-sharing (2C) complexes and the monodentate mononuclear corner-sharing (1V) complexes were present on the surface of the As(III)-treated samples under high surface coverage conditions (Γ = 1.0−12.2 μmol/m2). However, more Fe atoms were coordinated with each As atom for the monodentate mononuclear complexes in the As(V)/As(III)-treated siderite under oxic conditions (1.8 ± 0.5 and 2.2 ± 0.5, respectively) than those in the As(V)/As(III)treated siderite under anoxic conditions (1.0 ± 0.5 and 0.9 ± 0.5, respectively) and the As(V)/As(III)-treated goethite (1.1 ± 0.5 and 0.9 ± 0.5, respectively) (Table 2). The more Fe atoms coordinated with As atom in the monodentate complexes would be related to the higher adsorption capacity of the As(V)/As(III)-treated siderite under oxic conditions. Besides, for the bidentate binuclear complexes, more Fe atoms were observed to be coordinated with each As atom in the As(V)/ As(III)-treated siderite under oxic conditions (2.5 ± 0.5 and 3.2 ± 0.5, respectively) than those in the As(V)/As(III)-treated siderite under anoxic conditions (2.0 ± 0.5 and 1.8 ± 0.5, respectively). Accordingly, the coexistence of siderite-goethite bimineral during the mineral transformation in As-siderite system under oxic conditions was expected to result in the great number of Fe atoms coordinated with As atom in both 1V complexes and 2C complexes. Application. Enhancement of As adsorption on bimineral adsorbent during partial mineral transformation from siderite to goethite was evaluated by using modified natural siderite. The objective of modification was to create the coexistence of

Figure 6. EXAFS spectra (a) and their Fourier transforms (b) of As(V)-treated siderite (oxic), As(V)-treated siderite (anoxic), and As(V)-treated goethite (oxic). Solid lines represent the experimental EXAFS and radial structure function data, and dotted lined are the fits derived from the theoretical EXAFS function in Artemis.

Figure 7. EXAFS spectra (a) and their Fourier transforms (b) of As(III)-treated siderite (oxic), As(III)-treated siderite (anoxic) and As(III)-treated goethite (oxic). Solid lines represent the experimental EXAFS and radial structure function data, and dotted lines are the fits derived from the theoretical EXAFS function in Artemis.

generally corresponding to the expected As(V)−O distance. It suggested that As(III) was oxidized to As(V) during adsorption on siderite under oxic conditions. The first coordination shell surrounding As in the As(III)-treated siderite under anoxic conditions and As(III)-treated goethite under oxic conditions was satisfactorily fit by 2.8−2.9 oxygen atoms at an As−O distance of 1.76−1.78 Å (Figure 7 and Table 2), closely corresponding to the As(III)−O distance (i.e., 1.79 Å in the AsO3 pyramidal molecule). It indicated that As(III) was not oxidized to As(V) in the siderite system under anoxic conditions and in the goethite system under oxic conditions. The results were in good agreement with reports by Jönsson and Sherman,23 Ona-Nguema et al.,27 and Manning et al.25 The second neighbor contributions to the EXAFS data were fit using As−Fe pairs at various distances and a multiple scattering (MS) contribution corresponding to the As−O−O− 1014



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the National Basic Research Program of China (the 973 program, No. 2010CB428804), the Program for New Century Excellent Talents in University (No. NCET-07-0770), and the Fok Ying-Tung Education Foundation, China (Grant No. 131017). The authors would like to thank the Shanghai Synchrotron Radiation Facility (Beamlines BL14W1 and BL15U1) and its staff (Z. Jiang, S. Zhang, X. Yu, and A. Li) for allowing us to perform the EXAFS and XANES analyses. Geomicrobiology Laboratory in China University of Geosciences (Beijing) was acknowledged for providing the access to the anaerobic chamber. Constructive comments from three anonymous reviewers are much appreciated.

siderite and goethite in the adsorbent. Although As adsorption on modified natural siderite was comparable to that on natural siderite with the initial As(III) concentration 1.0 mg/L (S2 in the Supporting Information). The adsorption capacity of modified siderite calculated from Langmuir isotherm fitting was around 2.68 mg/g, which is much higher than that of natural siderite (0.32 mg/g). Although adsorption capacity of synthetic siderite for As(III) under oxic conditions (around 115 mg/g) was higher than that of modified natural siderite under oxic conditions, the grain size of synthetic siderite (around 100 nm) is much smaller than modified siderite (0.5−1.0 cm), and initial As concentrations are higher in the experiments of synthetic siderite (2 to 600 mg/L) than in the experiments of modified siderite (0.2 to 10 mg/L), which would greatly increase As adsorption on the solids. The modified siderite with the grain size between 0.5 and 1.0 cm has a great advantage for column filter application due to its high permeability. Besides, adsorption capacity of modified siderite for As(III) was higher than ferric hydroxide granular (2.3 mg/g),42 granular activated carbon (0.09 mg/g),43 natural siderite (1.04 mg/g with grain size 0.25−0.5 cm),11,45 and natural hematite (0.20 mg/g).44 Since As removal by modified siderite was carried under oxic conditions with the contact time of 48 h (being 8 times in the experiments of synthetic siderite under oxic conditions) at room temperature, the mineral transformation did not occur for modified siderite samples during adsorption reactions. Although the Fe(II)−Fe(III) bimineral was formed for the modified siderite prior to As adsorption and for synthetic siderite during As adsorption, the Fe(II)−Fe(III) bimineral was believed to be the key material for As retention in these two systems. Therefore, it confirmed that bimineral coexistence during mineral transformation from siderite to goethite greatly improved As adsorption capacity of the adsorbent. This observation can be applied to modification of natural siderite which efficiently removed As from water solutions. Dong et al.38 and Muñiz et al.39 also found high removal efficiencies for As in the Fe(II)−Fe(III) systems, which may also be dependent on the coexistence of Fe(II) and Fe(III) minerals.

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ASSOCIATED CONTENT

S Supporting Information *

Detailed description of materials, batch experiments, sample analysis and data evaluation, distances of As−Fe and number of Fe atoms in As−Fe shells of As-treated minerals (S1), As adsorption on natural siderite and modified natural siderite (S2). This material is available free of charge via the Internet at http://pubs.acs.org.

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REFERENCES

AUTHOR INFORMATION

Corresponding Author

*Phone: +86-10-8232-1366. Fax: +86-10-8232-1081. E-mail: [email protected]. Corresponding author address: School of Water Resources and Environment, China University of Geosciences, Beijing 100083, P. R. China. Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS The study has been financially supported by National Natural Science Foundation of China (Nos. 41222020 and 41172224), 1015



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Enhancement of Arsenic Adsorption during Mineral Transformation

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