the iron oxides as arsenic removal media from water

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_______________________________________________________________________ In: Iron Oxides: Structure, Properties and Applications ISBN: 978-1-62257-427-8 Editor: Arturo I. Martinez © 2012 Nova Science Publishers, Inc.

Chapter 8

THE IRON OXIDES AS ARSENIC REMOVAL MEDIA FROM WATER Karla I. Camacho1,2, Nicolaza Pariona1,4, Arturo I. Martinez1,2, , Román Castro-Rodriguez3, Sergio Martinez-Vargas4, Dale L. Perry5 and Pascual Bartolo-Pérez3 1

Recursos Naturales y Energéticos, Cinvestav Unidad Saltillo, Carr. Saltillo-Mty. Km. 13, Ramos Arizpe, 25900 México 2 Doctorado en Nanociencias y Nanotecnología, Cinvestav, México 3 Departamento de Física Aplicada, Cinvestav Unidad Mérida, Mérida, Yucatán, 97310 México 4 Instituto de Estudios Ambientales, Universidad de la Sierra Juárez, Ixtlán de Juárez, Oaxaca, 68725 Mexico 5 Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720, USA

ABSTRACT Iron oxides (IO’s) have been widely used for arsenic removal from water. Arsenic is a world-wide problem that has caused a range of diseases to the population that lives near polluted waters. Current technologies have scaled down the contamination level, b ut the problem remains, mainly in developing countries and rural areas. It is highly desirable to develop arsenic remediation technologies that are economically affordable and environmentally sustainable. This review discusses the importance of iron oxides for arsenic removal from water. The various iron oxide phases with different origins are discussed; e.g., hematites from both natural origins and theirs synthesis at the nanometer scale are discussed. The particular emphasis in arsenic adsorption on IO’s is because iron oxide minerals are ubiquitously distributed in Earth’s crust, and the synthesized 

E-mail: [email protected].

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Karla I. Camacho, Nicolaza Pariona, Arturo I. Martinez et al. counterparts can be prepared at low cost, even on small scales with non-sophisticated equipment.

1. INTRODUCTION Pollution of the Earth has increased rapidly since the beginning of the industrial revolution, promoting the raise of both environmental and health problems. Among contaminants, arsenic is of great concern. Arsenic is a ubiquitous element that ranks number 20 in abundance in the Earth's crust, the number 14 in seawater, and number 12 in the human body [1]. It has been used in medicine, in various fields of agriculture, electronics, and the metallurgical industry. It is now well known that consumption of As, even at low levels, can lead to carcinogenesis and other diseases [2]. This chapter discusses the role of iron oxides as used for arsenic removal; for its importance and recent developments a special attention is focused on iron oxide nanoparticles. In the first three sections, a panoramic review of arsenic’s induced health problems, their location around the globe, and their relationship to the chemistry of arsenic is discussed. For its low cost, Section 4 and 5 are focused on adsorption, a major arsenic removal mechanism; additionally, the effects of important parameters in natural waters on the adsorption process are discussed. In Section 6, the use of natural sources of hematite, magnetite and goethite in arsenic removal is discussed; the use of natural sources is important because of their low cost and availability of iron ores in different parts of the globe. Finally, Section 7 discusses the advantage of using iron oxide nanoparticles for arsenic removal. The importance of new properties acquired by IO’s with nanometer dimensions and low-cost preparation techniques are related to the potential use in arsenic removal.

2. HEALTH P ROBLEMS AND DISTRIBUTION OF ARSENIC In different parts of the world, arsenic concentration in fresh water represents a health problem, since this element is toxic in small quantities. Arsenic in water is imperceptible, because it does not present a particular color or taste. However, when it is consumed in determined amounts, intestinal problems are caused [3]; additionally, prolonged consumption develops a range of serious diseases such as skin discoloration [4], cancer of skin, kidney and lung [5], blood vessel diseases [6], high blood pressure [7], and reproductive disorders [8]. Countries such as India, Bangladesh, China, Mexico, New Zealand, Hungary, USA, Argentina, Chile, El Salvador, Peru, and Nicaragua have significant health issues related to arsenic in water [9]. In some of these countries, different technologies have been implemented for the reduction of arsenic levels in drinking water [9], and others are under development [10]. The arsenic concentration in natural waters ranges from less than 0.5 μg/L to values higher than 5000 μg/L [11]. The World Health Organization (WHO) determined that the maximum permissible limit of arsenic in drinking water should be no more than 10 μg/L. This limit has been adopted by several countries; however, some countries such as Mexico have set limits as high as 25 μg/L, levels which are permitted by local laws [12]. The high concentration of arsenic found in different types of water is mostly due to natural mechanisms [13]. However, human activities such as mining, use of arsenic compounds in agriculture, and combustion of fossil fuels have influenced the natural

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concentration of arsenic in water [14]. In the environment, the highest concentration of arsenic is found in ground waters because of partial rock dissolution and slow flows. Although high contents of arsenic in source rocks are not directly associated with high arsenic in groundwater [15]. Arsenic in ground waters is frequently associated with typical environments such as closed basins in semiarid and arid climates, and strong reducing aquifers originated from alluvium and geothermal areas. In northern Mexico and the southwestern USA, high concentrations of arsenic in water have been associated with both arid oxidizing environments and anthropogenic activities [15]. In the Mexican states of Chihuahua, Coahuila, and Durango, arsenic in groundwater ranges from 10 to 700 μg/L [12]. Otherwise, in river water and groundwaters of New Mexico, values as high as 600 μg/L have been reported [12]. In arid zones of Chile and Argentina, high oxidizing environments dominate; in the Atacama Desert, As concentrations as high as 21,000 mg/L have been found in groundwater. These very high concentrations have been related to the Tatio geothermal field [16]. The largest region of high arsenic groundwater exist in Argentina, where concentrations as high as 11,500 mg/L have been reported [17], with averages lying in the 42-255 mg/L range [15, 18]. In reducing environments of Bangladesh and India, the affected aquifers are generally shallow (150-200 m) are arsenic-unaffected with concentrations lower that 0.5 g/L. In Hungary, Romania [19], Taiwan, and China, high arsenic concentration is frequently found in deep artesian wells with a high reducing environment, where As (III) is the more abundant species [20].

3. CHEMISTRY AND MOBILITY OF ARSENIC The arsenic mobility water bodies is governed by a variety of factors, among which the solubility and chemical reactivity of different arsenic species in water and interaction of these species in solution with the surfaces of minerals in contact with waters [21]. Arsenic is a metalloid that exhibits the following oxidation states -3, 0, +3 and +5. Arsenic in its pure form is not soluble in water. However, when it is combined with other elements such as oxygen, the oxidation states +3 and +5 are the most common in nature [1]. As (III) forms hard acids and As (V) forms soft acid species. In aqueous systems, the pentavalent species dominates on surface waters (aerobic environments), while the trivalent arsenites predominate in anaerobic environments such as groundwater [1, 12]. Frequently, inorganic forms of arsenic are present in water deposits. The arsenic species depend on pH, redox potential and microbial activity of the medium. The H2 AsO4- dominates at low pH (below 6.9) in oxidizing conditions. While the dominant species at high pH is HAsO42-. Under reducing conditions at pH ≤ 9.2, H3AsO4 formation predominates. Figure 1 shows the predominant area diagram for arsenic species. In the figure, it can be seen that the species of As (III) is neutral, while As (V) is negatively charged in the pH range between 4 and 10. This makes the As (III) more difficult to remove from the water by almost all known removal methods [2].

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Figure 1. Pourbaix diagram for arsenic at 25°C. Diagram determined with the Medusa software package. Please see: http://www.kemi.kth.se/medusa/.

Aquatic reducing environments are typical of regions with high organic matter content. Under these conditions, it is easy to find microorganisms and hence low oxygen concentrations. These environments may also contain high concentrations of sulfides, with subsequently low concentrations of dissolved arsenic. This explains how microorganisms reduce sulfates to provide the necessary conditions for arsenic sulfide precipitation [22]. Aquatic environments with high oxidation capacity are found in arid or semi-arid environments with high evaporation rates, high salinity and high pH. Therefore, the presence of soluble arsenate (AsO42-) is very common in oxidizing regions.

4. ARSENIC REMOVAL TECHNOLOGIES The arsenic removal methods recognized by the U. S. Environmental Protection Agency (EPA) are coagulation, adsorption, ion exchange and separation by membranes [23]. The selection of the method depends on arsenic speciation, hardness, presence of other chemical species such as silica, sulfate, phosphate, and iron, volume to be treated, degree of sophistication of the technique, and cost [24]. These technologies work well for As (V) removal, because it is easier to remove. In adsorption processes, the negative charge of As (V) species at pH greater than ~2.2 permits them to be electrostatically attracted to positively charged surfaces of metal hydroxides [25]. In contrast, As (III) exhibits neutral charge at pH below ~9.3; it decreases the removal efficiency by typical techniques. Therefore, the oxidation of As (III) is recommended as a previous step before the arsenic removal procedure [26].

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4.1. Adsorption One of the methods adopted for removing arsenic in water is adsorption. This technology is simple, does not require the use of poisonous chemicals, and adsorbents can be handled by final users at home or small communities [1]. Many adsorbents have been proven for arsenic removal such as iron oxides and oxyhydroxides [25], aluminum oxide [27], titanium dioxide [28], cerium oxide [29], and zero valence metal particles [30], as well as biomass (plants, food waste, mushrooms, proteins) and organic materials such as resins [1]. For the application of a technology for removal or mitigation of arsenic, important factors should be considered. In developing countries, it is preferred that the use of low cost technologies with removal efficiencies near or superior to the permissible arsenic limit [1, 2, 12, 24, 31] should be the technology of choice. In most cases adsorption does not require previous treatment steps, and operating costs are relatively low [1, 24]. Adsorption is a low-cost procedure and mentioned by the EPA as one of the best techniques for the removal of As. Adsorption is the most viable method for application in developing countries, where economic conditions and infrastructure are limited. Among adsorption materials, activated alumina has been successfully applied at slightly acid pH (5-7), giving removal efficiencies of ~95% for both As (III) and As (V) [32]. Iron oxyhydroxides such as akaganeite have proven to be a good material capable of removing As (V) and As (III) [33]. Additionally, combinations of materials such as the introduction of iron oxyhydroxide nanoparticles within a polymer network of an ion exchange resin have been used [1]. Additionally, some technologies have been developed that use very cheap materials such as sands coated with metal oxides, mainly iron oxides [34].

5. IRON OXIDES MATERIALS AND THEIR INTERACTION WITH ARSENIC IN WATER Amorphous iron oxyhydroxides (FeOOH), ferrihydrite and goethite are materials able to remove both As (III) and As (V) as well as methylated arsenic species from water [35]. Among iron oxide materials used for arsenic adsorption, one finds natural or synthesized powders and doped iron oxides. The adsorption capacity depends largely on the physical and chemical characteristics of the materials involved, including particle size. While natural iron oxides have particle sizes generally large, synthetics are commonly of nanometer sizes, and therefore have a greater surface area. Generally, the modification of iron oxides is focused on the achievement of larger surface areas for the generation of more active sorption sites [36]. The adsorption does not depend exclusively on the characteristics of the adsorbent itself. In aqueous media, variables such as pH, concentrations of other ions in water and the ionic strength are factors that are directly involved in the interaction of soluble species with the surface of the adsorbent.

5.1. Effect of pH

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The pH is one factor that affects the interaction of the adsorbents with species in aqueous solution. The optimum pH value for each adsorbent mainly depends on the pH of the point of zero charge (PZC). At pH lower than this value, the adsorbent surface becomes positive and negative if the pH is greater. Arsenic species dissolved in water exhibit negative charges; the arsenic species then should be attracted to positively charged adsorbents. At pH below 1, where As species are commonly neutral, arsenic cannot be absorbed. At these low pH values, iron oxides are dissolved and release the adsorbed species [37]. Some authors determined PZC values between 7.4 and 8.7 for pure iron oxide minerals; Shipley et al. reported that the values of PZC for hematite range from 5.5 to 9.3 [38] and from 6.4 to 7.2 for magnetite [39]. Table 1 summarizes PZC values of several iron oxides obtained from natural and synthetic sources. Table 1. PZC values, surface area, average particle size, and adsorption capacities for several natural and synthetic iron oxides Mineral

pH on Point Surface Zero Change Area (PZC)

Reference

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Average Particle As (V) Size Adsorption Capacity (mg/g) 18.4 nm 16.7

Commercial maghemite Sol-Gel maghemite

7.5 5.7

90.4

12.1 nm

25

[40]

Mechanochemical maghemite Commercial maghemite Commercial magnetite Synthetic magnetite Natural magnetite Natural goethite Goethite Goethite Goethite Goethite Goethite Natural hematite Natural hematite Commercial hematite Hematite Synthetic ferrihydrite Ferrihydrite Akaganeite

5.7

203.2

3.8 nm

50

[40]

7.5

60

20-40 nm

3.71

[41]

6.8

60

20-40 nm

3.71

[39]

6.2 6.5 6.8 9.3 9.2 8.5 9.3 8.7 6.7 8.1 6.8

98 0.89 2.009 54 27.7 70.8 43.7 0.381 1.66 31.7

10 µm 37 nm

24.55 ----20.7 ---

[29, 42] [43] [43] [37] [44] [45] [44] [44] [43] [46] [38]

8.5 8.5

600

-

--

[37] [44]

8.5 7.3

330

2.6 nm

120

[47] [33]

[40]

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5.2. Effect of Other Ions It has been found that iron oxides have chemical affinity with different chemical species such as arsenates, arsenites, phosphates, silicates, carbonates, and sulfides [48, 49]. In natural environments, the aqueous arsenic species are in contact with different dissolved species including carbonates, phosphates, silicates, chlorides, among others. During As adsorption, there is a competition for the iron oxide active sites with other anions. Phosphates are highly competitive with As (V) due to intrinsic affinity with the iron oxides [42, 48]. For different iron oxide phases, these ions affect the adsorption of arsenic as follows: hematite < goethite < ferrihydrite. Although phosphates are highly competitive, this competition can be diminished if the arsenic concentration is greater; an additional recommendation is to increase the amount of iron oxides for the adsorption process [42]. Sulfates compete strongly for adsorption sites with As (III) and to a lesser extent with As (V) at pH of 4-7 [42]. In particular, sands coated with iron oxides decreases the adsorption of arsenites in presence of sulfates [50]. Silicates have negative effects on the adsorption of As on iron oxides in general [42, 50]. In the case of goethite, it is believed that the surface potential decreased the As adsorption [50]. However, this negative effect can be reduced if adsorption is carried out at a pH of approximately 5 [42]. Dissolved organic matter and fulvic acid do not significantly affect the adsorption of arsenates on iron oxides. However, in the case of ferrihydrite, there is a considerable decrease in the adsorption of arsenites [50]. In ferrihydrite, the order of competitive attraction for different ions is as follows: phosphates > carbonates > sulfates > chlorides [51]. According to the study by Frau et al. [51], the adsorption of As (V) decreases with the presence of phosphates in a pH range of 410 and in the presence of bicarbonate at pH 8.3. On the other hand, silicates form strong bonds with iron oxides, presenting a strong influence on the adsorption on ferrihydrite. Additionally, the presence of silicate is known to inhibit the transformation of ferrihydrite to goethite [42]. In hematite, the order of competitive ability of ions is as follows: phosphates > silicates > carbonates > sulfates > nitrates [52]. It has been observed that most interfering ions are phosphates and silicates at concentrations of ~0.001 M, while sulfates, nitrates and carbonates affect the adsorption at concentrations ~0.01 M [53]. While with magnetite, ions which have significant effects on the adsorption of arsenic species are phosphates, bicarbonates and silicates at high concentrations. Calcium and magnesium ions, which give hardness to water, have no influence on As adsorption on magnetite [50]. Ions considered as contaminants in drinking water such as Cd2+ and chromates interfere on the arsenic removal, but these species can be removed simultaneously with As (III) and As (V) on goethite [42].

5.3. Effect of Ionic Strength For the case of arsenic adsorption on akaganeite, it was observed that the adsorption capacity of As (V) seems favored with increasing ionic strength (IS). In presence of KNO3, it was concluded that K+ ions exert cooperative effects with the adsorbent [33]. Similar results

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were found for batch tests with natural iron oxide minerals (mixtures of hematite and goethite) with the same type of electrolyte at pH of 7-12 [42]. Using NaNO3 as the electrolyte, no significant effects were observed in arsenic adsorption with increasing ionic strength on goethite and hematite [46]. Furthermore, Shipley et al. [50] reported that increasing ionic strength on magnetite, the adsorption of As (V) and As (III) is reduced if KNO3 is the electrolyte. This was attributed to the decrease in the electrostatic double layer around magnetite nanoparticles [50].

6. NATURAL IRON OXIDES Oxides and iron oxyhydroxides are formed naturally, depending on atmospheric conditions. The spatial arrangement of the Fe, O and H form multiple spatial arrangements, thus giving physical and chemical properties characteristics of each phase [54]. Iron oxides reported for As removal are magnetite, maghemite, goethite, akaganeite, ferrihydrite, lepidocrocite and hematite. Natural sources of iron oxides have been widely utilized for As removal [42, 43, 55]. Gimenez et al. [43] studied the adsorption of As (III) and As (V) on hematite, magnetite and goethite obtained from natural sources. The results show that the three phases are capable of adsorbing both arsenic species. But better performance was exhibited by hematite for As (III) removal, even though its surface area is smaller with respect to magnetite and goethite. Additionally, it was found that goethite can be used in a broader pH range (5-9), while magnetite works better at high pH with a limit of around pH = 9. Guo et al. [55] used natural hematite and siderite minerals for As removal. This work involved both packed columns and batch studies for the adsorption of dimethylarsinic acid (DMA), As (III) and As (V). In general, the natural siderites eliminated As from water more efficiently than the natural hematites. The pH generally had a great impact on arsenate removal by both the siderites and the hematites, while arsenite removal was slightly dependent on the initial pH. The adsorption capacities between hematite and siderites varied considerably. Hematite showed an adsorption capacity of 0.202 mg/g for As (V) [55]. Zhang et al. [42] used natural iron oxides mainly composed of hematite and goethite. This paper reported the adsorption of As (V) in concentrations lower than 1 mg/L at pH 4.56.5, obtaining adsorption capacities of 0.4 mg of As (V)/g of mineral. They considered the effect of KNO3, which allows an improvement of As (V) adsorption in alkaline solutions at pH of 7-12. The improvement was attributed to the decrease of negative charges on the minerals surface. The advantage of using natural iron oxides is its economic viability. On the other hand, the main disadvantage of using natural sources is fluctuation of particle size and low adsorption capacity. It has been reported that natural iron oxides exhibit large particle sizes, 0.25-0.5 mm for hematite [55]. However, the advantage of using large particle size is the easiness to be recovered after the adsorption process.

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7. IRON OXIDE NANOPARTICLES The use of iron oxides nanoparticles (NP’s) acquires importance, because they have a surface area greater than microparticles. The increase in surface area generates a large number of active adsorption sites. Besides the increase of surface area, another advantage is that they can be homogeneously dispersed in aqueous solution; this favors the mass transport towards the NP’s surface [56]. For As adsorption, most of the works have been focused on NP’s of magnetite and maghemite because of their peculiar magnetic properties, which allow NP’s recovery using external magnetic fields. The use of magnetic fields allows an effective and rapid recovery of fine powders after arsenic removal. In this section case studies reported for use of the different phases is discussed. Maghemite NP’s synthesized by different techniques have been applied in As (V) removal, with the initial concentrations ranging from 1 to 11 mg/L [40]. The synthesis techniques were decisive in the NP’s arsenic adsorption properties. Maghemite NP’s were synthesized by mechanochemical and sol-gel; also, commercial NP’s were evaluated. The highest adsorption capacities were at low pH (~3) and decreased as pH increased. The mechanochemically synthesized maghemite displayed better results with an adsorption capacity of 50 mg/g, followed by sol-gel prepared maghemite with 25 mg/g, and, finally, the commercial maghemite with 16.7 mg/g. It has been reported that maghemite NP’s can also be used for Cr (VI), Cu (II) and Ni (II) removal [57]. In a intent to use commercial pure magnetite NP’s, Chowdhury et al. [41] employed batch experiments using a mixture of magnetite/maghemite NP’s for As (III) and As (V) removal; the size of the used particles were between 20-40 nm. The adsorption capacity was 3.71mg/g for As (V) and 3.69 mg/g for As (III). Equilibrium was reached in 3 h at room temperature with an initial concentration of arsenic of 2 mg/L. Additionally, Shipley et al. [50] performed studies with commercial magnetite NPs with particle sizes of 20 nm. The initial concentrations of arsenates and arsenites used were 1 mg/L. Using batch experiments, 0.5 g/L of magnetite NP’s were added at pH 8 for 1 h, reaching adsorption capacities of 4.85 mg/g for As (V) and 5.12 mg/g for As (III). On the other hand, the effects of other ions such as phosphates, bicarbonates and silicates were evaluated, ions which lower the As adsorption capacity. An important parameter for arsenic removal is the particle size of the NP’s. Some authors have studied the effect of particle size of magnetite NP’s on As (III) and As (V) removal [56]. The range of particle size has been wide and ranges from 300, 20 and 12 nm; the role of the particle size on the arsenic adsorption was evaluated. Using concentrations of 0.5 g/L of magnetite NP’s, initial As concentration of 5 mg/L at pH 8 with a 0.01 M NaNO3 electrolyte, the results demonstrated that higher As (III) and As (V) adsorption was obtained with smaller NP’s. The adsorption capacities for 12 nm particles were 9.922 mg/g for As (III) and 9.844 mg/g for As (V), whereas for particles of 300 nm, the capacities were 2.486 and 2.918 mg/g for As (III) and As (V), respectively. In order to reach lower cost and an alternative way for iron oxide NP’s preparation, an innovative method which includes household substances and cookware has been proposed [58]. It includes olive oil, vinegar, drain cleaning agents and rust, and demonstrated that magnetite NP’s can be obtained with particle sizes ranging from 12 to 50 nm with low

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production costs. Finally, the authors mentioned that 15 g of these NP’s can remove 5 mg/L of arsenic from 50 L of water, while for removing the same amount of As, a mass of 1.4 kg of bulk magnetite is needed. Arsenic removal properties of hematite nanoparticles have been also considered. Hematite-coated magnetite nanoparticles have shown superior As removal characteristics than surfactant coated ball-milled magnetite nanoparticles [59]. The maximum arsenic adsorption capacity reported was 2.1 g/mg, and it was able to decrease the As concentration in water below the WHO regulations [59]. Small hematite nanoparticles of approximately 4-5 nm have been synthesized inside NaCl self-formed cages; these particles have shown higher surface areas and superior adsorption properties than hematite particles [60].

CONCLUSION Iron oxides are an excellent alternative for arsenic remediation. The use of iron oxides ores is a good procedure for water treatment, but their low surface areas may generate great amounts of residual adsorbents. On the other hand, synthesized iron oxide nanoparticles open the possibility of using less amount of materials, controlling the surface properties, and increasing the duration of the adsorbency. Finally, new methods for preparation of iron oxide nanoparticles are under development, they will improve the adsorption properties and decrease the cost of nanoparticles.

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