Water quality at eight points on the agricultural canals
\\n\\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\\n\\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'IntechOpen is proud to announce that 179 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\nThroughout the years, the list has named a total of 252 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\nReleased this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\n'}],latestNews:[{slug:"stanford-university-identifies-top-2-scientists-over-1-000-are-intechopen-authors-and-editors-20210122",title:"Stanford University Identifies Top 2% Scientists, Over 1,000 are IntechOpen Authors and Editors"},{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"},{slug:"all-intechopen-books-available-on-perlego-20201215",title:"All IntechOpen Books Available on Perlego"},{slug:"oiv-awards-recognizes-intechopen-s-editors-20201127",title:"OIV Awards Recognizes IntechOpen's Editors"},{slug:"intechopen-joins-crossref-s-initiative-for-open-abstracts-i4oa-to-boost-the-discovery-of-research-20201005",title:"IntechOpen joins Crossref's Initiative for Open Abstracts (I4OA) to Boost the Discovery of Research"},{slug:"intechopen-hits-milestone-5-000-open-access-books-published-20200908",title:"IntechOpen hits milestone: 5,000 Open Access books published!"},{slug:"intechopen-books-hosted-on-the-mathworks-book-program-20200819",title:"IntechOpen Books Hosted on the MathWorks Book Program"}]},book:{item:{type:"book",id:"1666",leadTitle:null,fullTitle:"Advances in Spatial Planning",title:"Advances in Spatial Planning",subtitle:null,reviewType:"peer-reviewed",abstract:"Spatial planning is a significant part of geosciences that is developing very rapidly. 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During his doctoral studies, Dr. Sayago tackled the problem of achieving low-voltage organic transistors employing electrolytes as the gating medium. His research contributed to shedding light on fundamental physicochemical processes in electrochemical transistors and energy storage devices. After his PhD studies, Dr. Sayago worked as a consultant for Bowhead Health Inc., a Canadian startup company aiming for the commercialization of bioelectronic devices for preventive medical applications. His team designed and built a biosensor device capable of testing 50 µl of blood which led the company to secure a private funding from the world-class Mexican company Grupo Arcoiris. As a Postdoctoral Researcher at the Institute of Renewable Energies, UNAM, Dr. Sayago investigates biocompatible and biodegradable electrodes engineered for energy storage and heat transfer applications. 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However, P is difficult for plants to obtain from the rhizosphere and P deficiency is one of the major limitations on crop production. This is because soluble P in soil, the primary P source for plants, is extremely low concentration (Condron et al., 2005) and significant portions of P in the soil are various organic complexes and unavailable (Raghothama, 2005). On a worldwide scale, land covering 5.7 billion hectares is estimated to be deficient in P for optimal crop production (Batjes, 1997). Since the soluble P in the soil is easily taken up by plants and microorganisms, continuous application of P fertilizer is necessary for crop production.
\n\t\t\tThe global demand for P has increased 10-fold since the beginning of the 20th century (Cordell et al. 2009) and approximately 80% of the demand is for agricultural fertilizers (Steen, 1998). Thus, more P will be required as the world’s population increases. However, there is concern that world P resources will be depleted in the next 50–100 years, because the reserves of high-grade phosphate rock are limited (Runge-Metzger, 1995; Steen, 1998; Smil, 2000; Stewart et al., 2005). Therefore, the recovery of P is essential for sustaining food production.
\n\t\t\t\n\t\t\t\tFigure 1 shows a conceptual illustration of the global P cycle, which is completed by P flux from the ocean to the land, and is intimately linked to global ocean circulation. The P derived from weathering or fertilizer application on the land is washed down in rivers and enters the ocean food chain. In deep ocean water (about 2,000–3,000 m in depth), the P concentration is considerably higher than that at the surface because dead fish and plankton fall on the ocean floor. However, the P-rich water is too deep for humans to exploit. In the deep ocean, the water flows from the Atlantic Ocean to the Pacific Ocean via the Antarctic and the Indian Ocean, while the surface water flows in the opposite direction. This movement is very slow; about 2000 years is required to complete this circulation. In some areas of the Pacific Ocean, the flow rises from the bottom to the surface, but this is rare phenomenon. Because the occurrence of this rising flow depends on a complex combination of sea currents, winds, and geographical features. Consequently, these selected areas are abundant in plankton and fish. However, the P flux from ocean to land occurs only via fishery and seabirds’ droppings (guano), unlike nitrogen that can be released into the atmosphere via denitrification. In addition, the seabed is gradually transformed into land by the geological movement of the Earth\'s crust, but this occurs on a much longer time scale than do human activities. Therefore, the global P cycle is extremely limited.
\n\t\t\tConceptual illustration of the global P cycle (data from Sumi, 1989)
Despite the limited nature of the P cycle, repeated applications of fertilizers and organic matter builds up nutrients in the soil. Strong relationships between the level of P monitored by soil tests and the amount of P lost in runoff have been reported (Pote et al., 1996; Sharpley, 1995). Thus, excessive application of P fertilizers contributes to eutrophication, which is sometimes responsible for the lack of clean water resources. From this viewpoint, the recovery of P is also essential.
\n\t\t\tThe behavior of P in nature has been affected by iron (Fe) oxides since ancient time (Bjerrum & Canfield, 2002). In natural water bodies such as canals, swamps, and ponds with low oxygen groundwater seeps and circumneutral conditions, the accumulation of soft, reddish-brown sediment is often observed (Fig. 2). The essential compounds in this sediment are biogenic Fe oxides produced by microaerobic Fe-oxidizing bacteria (Emerson et al., 1999; Emerson & Weiss, 2004; James & Ferris, 2004) and this ferric substance in the sediment can adsorb P in a similar manner to abiotic P adsorbents of ferric compounds (Boujelben et al., 2008; Persson et al., 1996; Seida & Nakano, 2002; Zeng et al., 2004). Therefore, biogenic Fe oxides in nature are considered as one of the P resources. However, they have not yet been recognized as such, although they have been used for ferrous Fe removal in water treatment facilities (Pacini et al., 2005; Katsoyiannis & Zouboulis, 2004; Søgaard et al., 2001). This is because biogenic Fe oxides in natural water bodies are easily dispersed by water turbulence. In addition, it is difficult to collect only the Fe oxides as a P resource, because they usually accumulate only a few centimetres, and anaerobic and malodorous mud exists underneath (see Fig. 3). Moreover, the mud deposits that have existed for a long time may accumulate harmful substances such as heavy metals.
\n\t\t\tAccumulation of reddish–brown soft sediment in an agricultural canal
Conceptual illustration of P recovery from natural water bodies using Fe-oxidizing bacteria and woody biomass.
A new method for the recovery of P from natural water bodies using Fe-oxidizing bacteria and woody biomass as a carrier has been proposed (Fig. 3). A woody carrier is immersed in water in which Fe-oxidizing bacteria are abundant and then removed several weeks later. In this chapter, this method was tested in an agricultural area, dominated by rice paddy fields, located in the eastern part of Shimane Prefecture, Japan. As the woody carrier, sawdust from the Japanese cedar and Japanese cypress were used. Since the accumulation of biogenic Fe oxides was observed throughout the year at several locations, the water quality at these points was monitored. In addition, heavy metals on the immersed carrier were also measured, because biogenic Fe oxides have the potential to also adsorb heavy metals such as arsenic (As), cadmium (Cd), chromium (Cr), mercury (Hg), lead (Pb), zinc (Zn), and nickel (Ni).
\n\t\tSamples for water quality monitoring were collected at eight points on agricultural drainage canals (Fig. 4) on December 13, 2008. These points were located in the downstream area of the Hii River, Japan, at approximately 35° 24′ N and 132° 50′ E. The pH and oxidation-reduction potential (ORP) were monitored with a portable analyzer (Kasahara Chemical Instruments, KP-5Z). The Fe, P, and nitrogen (N) concentrations were analyzed in accordance with Japanese Industrial Standard (JIS) K 0102 (Namiki, 2003): total Fe (T–Fe) and dissolved Fe (D–Fe) were measured by the 1,10-phenanthroline method; total phosphorus (T–P) was measured by the ascorbic acid reduction molybdenum blue method after potassium peroxodisulfate decomposition; phosphate phosphorus (PO4–P) was measured by the ascorbic acid reduction molybdenum blue method; total nitrogen (T–N) was measured by UV absorption spectroscopy after alkaline potassium peroxodisulfate decomposition; ammonium nitrogen (NH4–N) was measured by the indophenol blue method; nitrate nitrogen (NO3–N) was measured by ion chromatography (Shimadzu HIC–6A). The total organic carbon (TOC) concentration was measured by Shimadzu TOC-Vcsn system and suspended solids (SS) were measured by gravimetric analysis using glass-fiber filters (pore size = 0.45 μm; Advantec GS25).
\n\t\t\tAlthough the precise mechanism of Fe oxidation-deposition by Fe-oxidizing bacteria is not sufficiently understood (Pacini et al. 2005) and some of the species are characterized as autotrophic (Hallbeck & Pedersen, 1991; Imai, 1984), a substantial accumulation of biogenic Fe oxides was found on the surface of submerged aquatic plants in an agricultural drainage canal (Fig. 5). On the basis of this finding and some trial-and-error experiments, woody biomass (conifer heartwood) was used as the carrier for collecting biogenic Fe oxides. In particular, sawdust (particle size: 0.2–2 mm) of the Japanese cedar (Cryptomeria japonica) and the Japanese cypress (Chamaecyparis obtusa) were used, both of which are typical conifers found in Japan. The heartwood of the conifer contributes very little to secondary water pollution during the immersion test period, because it mainly consists of carbon, hydrogen, and oxygen and contains extremely small amounts of N and P (Jodai & Samejima, 1993). In addition, it contains a large amount of lignin, flavonoids, and phenols, which provide resistance to wood-decomposing fungi (Jodai & Samejima, 1993). Moreover, approximately 97% of the wood tissue of conifer heartwoods consists of tracheids, which are hollow elongated cells (Furuno & Watanabe, 1994). Thus, the sawdust is expected to have a large specific surface area.
\n\t\t\t\tMap of study site
Accumulation of biogenic Fe oxides on the surface of submerged aquatic plant
Sheathed bacteria, Leptothrix spp.
The immersion test was conducted in an agricultural drainage canal (at point 1 in Fig. 4) where reddish-brown sediment accumulated, and sheathed bacteria (Leptothrix spp.) were found to be abundant (Fig. 6). The test was performed during the irrigation period for paddy fields (from May to September 2009) and the non-irrigation period (from October 2009 to April 2010), because the canal is mainly fed by drainage water from paddy fields via surface outlets and underdrains, and the water quality is affected by the paddy field irrigation.
\n\t\t\t\tIn this test, the woody carrier was placed in a container of non-woven bag and lowered to the bottom of the canal. The carrier in the container was removed from the water after immersion for 4 weeks. The Fe collected on the immersed carrier was analyzed by the 1,10-phenanthroline method (Stucki & Anderson, 1981), and the P adsorbed on the Fe oxides was analyzed by the Bray-2 method (Byrnside & Sturgis, 1958). The Bray–2 P is a portion of the soil P and is one of the indexes of available P for plant uptake. In this study, the adsorbed P is expressed as g/kg instead of the conventional expression of Bray-2 P (mg P2O5/100 g dry material). In addition, the water samples were collected at weekly intervals and the water quality of D-Fe and PO4-P was analyzed by the above-mentioned methods.
\n\t\t\tElemental analysis of the immersed carrier was carried out by X-ray fluorescence spectrometry system (Shimadzu, EDX-720) at a voltage of 50 kV and a current of 1 mA.
\n\t\t\t\n\t\t\t\t\tTable 1 presents the water quality at eight points on the agricultural canals. At all points, the D–Fe concentration was much lower than the T–Fe concentration, and the same relationship was found between the PO4–P concentration and T–P concentration. Therefore, most of the Fe and P in the water were associated with particulate matter. The average concentrations of T–N and TOC were 2.864 and 2.180 mg/L, respectively, and the NO2–N concentration was much lower than the T–N concentration.
\n\t\t\t\t\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Water quality at eight points on the agricultural canals
Data plot on pH–OPR diagram (from Mouchet, 1992). Black dots represent the data monitored at the study sites of Fig. 4.
Biogenic Fe oxides (brown mass) on woody carrier
Since the Fe oxidation was characterized with a pH–ORP diagram (Mouchet, 1992), the data from this study were plotted on it (Fig. 7). In this diagram, the pH–ORP area is divided into physical-chemical oxidation, biological oxidation, and stability of ferrous Fe. The data from this study were within the range of pH = 6.7 to 7.1 and ORP = −0.03 to 0.05 V, and were located near the boundary between the biological oxidation and the stable ferrous Fe area. Since the suitable aquatic conditions for the growth of Fe-oxidizing bacteria have been reported to be low concentration of oxygen and circumneutral pH (James & Ferris, 2004), the results of present study agree with this knowledge.
\n\t\t\tThe color on the woody carrier changed from light yellow to dark brown. Observation using a microscope revealed that biogenic Fe oxides produced by Fe-oxidizing bacteria had accumulated on the woody carrier (Fig. 8(a)). In many cases, the woody carriers were not easily visible because they had been completely covered by a mass of Fe oxides (Fig. 8(b)).
\n\t\t\t\t\n\t\t\t\t\tFigure 9 shows the Fe collected on the woody carrier and the D-Fe concentrations of the water at the site of the immersion test. The average accumulation of Fe on the Japanese cedar was 7.91 g/kg during the irrigation period and 6.74 g/kg during the non-irrigation period. The respective values for the Japanese cypress were 7.67 and 5.54 g/kg. There were no significant differences between the values during the irrigation and the non-irrigation period. The average D–Fe concentration during the irrigation period (0.952 mg/L) was much higher than that during the non-irrigation period (0.338 mg/L). There were no significant differences during the irrigation and non-irrigation period between the collected Fe for the Japanese cedar and the Japanese cypress (Fig. 10). When these values are expressed in parts per million (ppm), the Fe collected during the irrigation period was 7,910 ppm for the Japanese cedar and 7,670 ppm for the Japanese cypress, while the D–Fe concentration was 0.952 ppm. Therefore, the concentration of the Fe on the woody carrier was 8,000- to 8,300-fold greater than the Fe dissolved in the water. For the non-irrigation period, the degree of Fe concentration was 16,000- to 20,000-fold greater.
\n\t\t\t\t\n\t\t\t\t\tFigure 11 shows the P adsorbed on the woody carrier and the PO4-P concentration. The average P adsorbed on the Japanese cedar carrier was 0.350 g/kg during the irrigation period and 0.187 g/kg during the non-irrigation period. The respective values for the Japanese cypress were 0.332 and 0.172 g/kg. The differences between the values during the irrigation and non-irrigation periods were significant (p < 0.05). The average PO4–P concentration of the water during the irrigation period (0.058 mg/L) was much higher than that during the non-irrigation period (0.022 mg/L). This is probably because the anaerobic conditions caused by flooded water on the paddy fields during the irrigation period lead to the reduction of ferric phosphate (FePO4) compounds and the release of Fe2+ and phosphate (PO4\n\t\t\t\t\t3-) ions. There were no significant differences in the adsorbed P during the irrigation and the non-irrigation period between the Japanese cedar and the Japanese cypress (Fig. 12). When these values are expressed in ppm, the P adsorbed during the irrigation period was 350 ppm for the Japanese cedar and 332 ppm for the Japanese cypress, while the PO4–P concentration was 0.058 ppm. Therefore, the concentration of the P on the woody carrier was 5,700- to 6,000-fold greater than the P dissolved in the water, and for the non-irrigation period, it was 7,800- to 8,500-fold greater.
\n\t\t\t\tFe content after the immersion test. (a), (b): collected Fe after 4 weeks immersion; (c): D-Fe concentration of the water (means and standard errors, n=8)
Comparison of collected Fe between Japanese cedar and Japanese cypress (n=8)
P contents from the immersion test. (a), (b): adsorbed P after 4 weeks immersion; (c): PO4–P concentration of the water (means and standard errors, n=8)
Comparison of adsorbed P between Japanese cedar and Japanese cypress (n=8)
P fertility of the immersed carrier in the relationship between the Bray-2 P in arable soils and the rice yield index (adapted from Komoto, 1984)
\n\t\t\t\t\tFigure 13 shows the P fertile position of the immersed carrier on the relationship between the Bray-2 P in arable soils and the rice yield index (adapted from Komoto, 1984). In low-fertility soil (Fig. 13(a)), the yield index increases with Bray-2 P, but does not increase over the fertile level of 0.025 g/kg of Bray-2 P. As shown in Fig. 13(b), soils containing greater than 0.1 g/kg are categorized as high-fertility soil. The P values from this study were between 8- and 17-fold higher than the required level (0.025 g/kg) and categorized in the range of high-fertility soil. Therefore, the immersed carrier had obtained sufficient P fertility.
\n\t\t\t\n\t\t\t\t\tFigure 14 shows an example of an X-ray fluorescence spectrum of the immersed carrier. Fe was the main species detected, although silicon (Si), calcium (Ca), aluminum (Al), P, sulfur (SO4), potassium (K), chlorine (Cl) were also present. Heavy metals were not detected on most of the carriers, but traces of Pb and Zn were detected in some samples (Table 2). However, they were well below regulation levels set out in the Fertilizers Regulation Act (Ministry of Agriculture, Forestry and Fisheries, 2007) and the Guidelines against Heavy Metal Accumulation in Arable Soil (Environment Agency, 1984). This was probably because the study site was in a rural area that had not been contaminated by heavy metals and also because the immersion period was too short for these metals to accumulate.
\n\t\t\t\tX-ray fluorescence spectrum of immersed carrier
\n\t\t\t\t\t\t\t\t | \n\t\t\t\t\t\t
Heavy metal concentrations in immersed carrier (maximum for n=45)
The findings reported in this chapter have been obtained from a specific region in Japan. However, Fe is the third most abundant metal found in the soil (Spark, 1995), and Fe-oxidizing bacteria are not rare (Emerson et al., 1999; Emerson & Weiss, 2004; James & Ferris, 2004). Thus, this method can be applicable in many places, provided suitable aquatic conditions supporting the growth of Fe-oxidizing bacteria (low concentration of oxygen and circumneutral pH) are available. In addition, the immersed woody carrier can be applied directly to agricultural land in the form of a fertilizer, without P extraction procedures, which are commonly required for P recovery methods. Therefore, this method is a low-cost technique that should contribute to P resource recycling and the improvement of the aquatic environment, if adopted on a large scale.
\n\t\t\tA new method of P recovery from natural water bodies using Fe-oxidizing bacteria and woody biomass (Japanese cedar and Japanese cypress) was applied in an agricultural canal during irrigation and non-irrigation periods. The amounts of P adsorbed on the carrier during these periods were 0.332–0.350 and 0.172–0.187 g/kg, respectively, while the PO4–P concentrations of the water were 0.058 and 0.022 mg/L. Expressed these values in parts per million, the P adsorbed on the carrier was 5,700- to 8,500-fold more concentrated than the P dissolved in water. The P on the carrier was 8- to 17-fold higher than the required level for sufficient fertility to support rice production, and it was categorized in the range of high-fertility soil. Some traces of heavy metals adsorbed on the carrier were detected, but they were much lower than the regulation levels. In addition, the woody carrier can be applied directly to agricultural land without P extraction. Therefore, this method is a low-cost technique that should contribute to P resource recycling and the improvement of aquatic environment.
\n\t\tThis study was partially supported by a grant from the Shimane University Priority Research Project and a Grant-in-Aid for Scientific Research from the Japan Society for the Promotion of Science (#20380179).
\n\t\tWater pollution is a concern for the European population, and the quality objectives for the water protection are set through the EU Water Framework Directive. Also, one of the targets of the Clean Water and Sanitation Goal within the Millennium Sustainable Development Goals of the 2030 Agenda is to achieve universal and equitable access to safe and affordable drinking water for all by 2030 [1].
\nThe challenges in treating drinking water are dependent on the water sources, mainly consisted of surface and groundwater. Problematic substances in the drinking water sources can include organic matter and/or different inorganic contaminants, e.g., nitrite, nitrate, and ammonium.
\nOne of the common and advanced unitary processes used in drinking water technology is sorption designed as activated carbon- or zeolite-based filtering. Due to more hydrophobic nature of the activated carbon, it has been recognized for elimination of a broad range of hazardous materials belong to the organic class from aqueous solutions. Activated carbon is less efficiently applied for removal of simple inorganic metallic ions or small-size anions [2].
\nZeolite is also a known filtering material that exhibits a high sorption capacity [3] characterized by a selectivity degree in relation with the type of zeolite based on its specific properties of molecular sieve and ionic exchanger [4, 5, 6]. The main disadvantage is represented by the fouling of the filtering material surface.
\nPhotocatalysis process is considered very promising for advanced water treatment based on the oxidation and reduction reaction for in situ generation of highly reactive transitory species (i.e., H2O2, OH, O2, O3) for mineralization of organic compounds and disinfection by-products [7, 8], through the electron-hole pair formation under UV or solar irradiation.
\nAmong various semiconductors that have been investigated in photocatalysis application, titanium dioxide (TiO2) has attracted much attention due to its physical and chemical stability, negligible toxicity, the resistance to corrosion, redox selectivity, high photostability, and easy preparation [3, 9, 10]. By UV irradiation onto TiO2 surface, under conditions of photon energy (hv) greater than or equal to the bandgap energy of TiO2, the electron will be photoexcited from the valence band to the empty conduction band leading to an empty unfilled valence band that corresponded to the hole and thus creating the electron-hole pair. The electron-hole pair is involved within various oxidative/reductive reactions including the degradation of organics.
\nFor the drinking water treatment, the main disadvantage of TiO2-based photocatalysis is given by the necessity of the further separation phase to remove TiO2 from water, in order to avoid the loss of catalyst particles and introduction of the new pollutant of contamination of TiO2 in the treated water [11]. A solution to avoid the introduction of a new separation phase includes catalyst fixation onto various supports, e.g., activated carbon [12] and mesoporous clays [13]. The catalyst immobilization on different supports allows getting catalyst composites, which are considered a new generation of catalyst with different properties in relation with those of solely TiO2. According to the obtaining methods, there are a large variety of composites [14], from which in this chapter will be discussed:
Composites with TiO2 coated (supported) on the support of activated carbon by the type of powder and granular and zeolite [15, 16, 17, 18, 19, 20, 21]
Hybrid composites, which comprise a matrix material of polymer (epoxy) in which TiO2 and the support of carbon nanotubes or nanofibers are dispersed [22, 23, 24]
In this chapter, two types of composites obtained by two different methods and applied in the drinking water treatment are presented:
TiO2 supported on powdered activated carbon (PAC-TiO2), granular activated carbon (GAC-TiO2), and zeolite (Z-TiO2), namely, supported TiO2.
TiO2 and multiwall carbon nanotubes and carbon nanofibers dispersed within epoxy matrix (CNT-TiO2-Epoxy, CNF-TiO2-Epoxy), namely, TiO2 composite. The carbon and zeolite components were selected taking into account their utility as sorbent for natural organic matter [20, 21, 22, 23, 24].
The granular, powdered activated carbon and natural zeolite were functionalized with TiO2 using titanium tetraisopropoxide (TTIP) as TiO2 precursors by sol-gel method (Figure 1).
\nSchematic diagram of obtaining PAC-TiO2, GAC-TiO2, and Z-TiO2.
For the synthesis process of the composite materials consisting of carbon nanotubes or carbon nanofibers mixed with TiO2 particles within epoxy matrix, the two-roll mill technique was applied (Figure 2).
\nSchematic diagram of obtaining CNT-TiO2-Epoxy and CNF-TiO2-Epoxy.
The morphology of all synthesized materials was observed by a scanning electronic microscope (SEM, Inspect S PANalytical model) coupled with the energy-dispersive X-ray analysis detector (EDX). Figure 3a–c presents SEM images for PAC-TiO2, GAC-TiO2, and Z-TiO2, which show the layered structure of activated carbon and a nonuniform distribution and more or less agglomeration of TiO2 nanoparticles onto the surface. It can be also seen that TiO2 only adhered to the surface of zeolite without the insight of the inside of the zeolite pores.
\nSEM images for (a) PAC-TiO2, (b) GAC-TiO2, and (c) Z-TiO2.
The results of semiquantitative elemental analysis of the synthesized material surface were presented by EDX spectra indicating Ti and C presence for PAC-TiO2 and GAC-TiO2 and, also, the presence of Ti on the natural zeolite (Figure 4). Small amounts of Al, Si, and S were identified within the activated carbon as both powdered and granular as impurities and the presence of K and Ca within the zeolite composition were found.
\nEDX spectra for (a) PAC-TiO2, (b) GAC-TiO2, (inset: GAC), and (c) Z-TiO2 (inset: zeolite).
For composite materials that used epoxy as matrix, it can be noticed that TiO2 nanoparticles were attached on the nanostructured carbon surface, and, also, a well dispersion of carbon and TiO2 nanoparticles within epoxy matrix is noticed (Figure 5a,b). A slight more uniform distribution of TiO2 nanoparticles seems to be for CNF in comparison with CNT [22]. The presence of TiO2 particles in composite materials was confirmed by EDX spectra (Figure 6).
\nSEM images for (a) CNF-TiO2-Epoxy and (b) CNT-TiO2-Epoxy.
EDX spectra for (a) CNF-TiO2-epoxy and (b) CNT-TiO2-epoxy.
X-ray diffraction measurements were carried out to determine the crystal phase composition using a PANalytical X’PertPRO MPD diffractometer. Figure 7 presents the XRD patterns of GAC-TiO2, PAC-TiO2, and Z-TiO2. The anatase form of TiO2 is the predominant phase, identified by diffraction lines at 2θ of 25.3, 38.6, 48, 54, and 62.97° [25]. Also, the XRD results revealed that the major component of natural zeolite used in this study is clinoptilolite (2θ ~ 10°; 12°; 22.5°; 30°) [26].
\nXRD pattern for PAC-TiO2, GAC-TiO2, and Z-TiO2.
Figure 8 presents the XRD patterns of composite materials based on nanostructured carbon. It is obviously the presence of anatase form of TiO2 as predominant phase, with the intensity of diffraction lines higher due to the higher TiO2 loading within the composite composition in comparison with the supported TiO2.
\nXRD pattern for CNT-TiO2 and CNF-TiO2.
Various types of carbon and zeolite are reported as good sorbents for various types of pollutants from water [2, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24]. The easy separation of these materials from water and their good sorption capacity that is important in the first stage of the overall photocatalysis process make them very promising as support for the TiO2 immobilization.
\nHumic acids (HAs) represent a main component of natural organic matter that gives the organic loading of drinking water sources, which must be removed or destroyed because of water quality regulations. Also, the presence of HAs before the chlorination step as disinfection could lead to trihalomethane and other toxic by-product generation. The efficiency of supported TiO2 materials for the sorption and the photocatalysis of HA from water, expressed as HA removal efficiency, is presented comparatively in Figure 9.
\nEvolution of HA removal efficiency by sorption and photocatalysis for 50 mg·L−1 HA onto (a) GAC-TiO2, (b) Z-TiO2, and (c) PAC-TiO2.
The HA removal efficiency was calculated using the following equation:
\nwhere C0 and Ct are the concentrations of HA in aqueous solution in terms of A254 at initial time and at any time t, respectively (mg·L−1).
\nThe sorption was assessed as the preliminary and compulsory step of the overall photocatalysis process taking into consideration also the possibility to use the supports as simple sorbents and only for self-cleaning to apply the photocatalysis. The sorption capacity for HA is better for PAC-TiO2, while the photocatalytic activity is better for GAC-TiO2. This should explain the morphological structure and the sizes of the particles. The lower particle size leads to the higher sorption capacity, while for the photocatalysis application the size of support decreased the photocatalytic activity may be due to the finer suspension should hinder the UV irradiation penetration to the TiO2 surface.The sorption and the photocatalysis capacities of TiO2 composite materials assessed in terms of HA removal efficiency showed the superiority of CNT-TiO2-Epoxy versus CNF-TiO2-Epoxy. It can be noticed that a slight photocatalytic activity was found for both materials (Figure 10).
\nEvolution of removal efficiency of 25 mg·L−1 HA using CNT-TiO2-epoxy by photocatalysis (a), sorption (b), CNF-TiO2-epoxy by photocatalysis (c), and sorption (d).
For HA removal, the sorption capacity of tested materials increased in order:
\nThe evaluation of photocatalytic activity after the sorption step showed an increasing order:
\nThese behaviors should be explained by the available sites of the carbon in the sorption process and the available sites of TiO2 in the photocatalysis process, which are in direct relations with the morphology, size, and the bonding type between TiO2, carbon, and zeolite support. Also, epoxy resin hindered the available sites, which decreased both sorption capacity and photocatalytic activity of TiO2 composite materials.
\nIn order to determine some mechanism aspects regarding the sorption and photocatalysis processes, several kinetic models must be checked to find the optimum one. Two different kinetic models are used to fit the experimental data, i.e., pseudo-first-order and pseudo-second-order kinetic models [27].
\nThe pseudo-first-order kinetic adsorption was suggested by Lagergren (1898) for the adsorption of solid/liquid systems. It can be expressed in integrated form as shown in Eq. (2):
\nwhere, k1 is the rate constant of adsorption (min−1) and qt is the adsorption loading of dye (mg·g−1) at time t (min).
\nThe pseudo-second-order kinetics, proposed by Ho and Mckay [28], is expressed in Eq. (3):
\nwhere, k2 is the rate constant of the pseudo-second-order adsorption kinetics (g·mg−1·min−1) and qe is the equilibrium adsorption capacity (mg·g−1).
\nPseudo-first- and pseudo-second-order kinetic models were tested for fitting the sorption and photocatalysis experimental data (Tables 1 and 2). The linear plots of t/qt vs. t show that the experimental data agree with the pseudo-second-order kinetic model for the HA adsorption. The calculated qe values agree very well with the experimental data, and the correlation coefficients for the pseudo-second-order kinetic model are higher than 0.90 in almost all cases. These indicate that the adsorption of HA from water onto materials obeys the pseudo-second-order kinetic model that predicts an exponential decay of concentrations as a function of time. The pseudo-first-order kinetic model was not appropriate for fitting the sorption experimental data, while the photocatalysis experimental data were fitted well with both kinetic models with the correlation coefficient higher than 0.90. However, there is a significant difference between calculated and experimental qe using the pseudo-first-order kinetic model that limits its interpretation (Table 2), and, thus, it means that the pseudo-second-order kinetic model is most appropriate. Besides the kinetic parameter, the pseudo-second-order kinetic model informed about the significance of the sorption step within the overall photocatalysis process. It is well known that the reaction rate and kinetics are influenced by many experimental parameters, e.g., HA concentration, catalyst dose, and pH [22].
\nCatalyst | \nParameters | \nAdsorption | \nPhotocatalysis | \n
---|---|---|---|
\n | \n | HA concentration (50 mg·L−1) | \n|
PAC-TiO2 | \nqe(mg*g−1) | \n38.34 | \n44.25 | \n
k2(g·mg−1·min−1) | \n0.0067 | \n0.0031 | \n|
R2 | \n0.915 | \n0.996 | \n|
GAC-TiO2 | \nqe(mg*g−1) | \n25.59 | \n49.78 | \n
k2(g·mg−1·min−1) | \n0.00381 | \n0.0170 | \n|
R2 | \n0.966 | \n0.998 | \n|
Z-TiO2 | \nqe(mg*g−1) | \n28.65 | \n42.32 | \n
k2(g·mg−1·min−1) | \n0.0059 | \n0.0025 | \n|
R2 | \n0.976 | \n0.985 | \n|
\n | \n | HA concentration (25 mg·L−1) | \n|
CNT-TiO2-Epoxy | \nqe(mg*g−1) | \n20.68 | \n19.98 | \n
k2(g·mg−1·min−1) | \n0.0024 | \n0.0015 | \n|
R2 | \n0.986 | \n0.996 | \n|
CNF-TiO2-Epoxy | \nqe(mg*g−1) | \n13.06 | \n12.37 | \n
k2(g·mg−1·min−1) | \n0.0045 | \n0.0001 | \n|
R2 | \n0.996 | \n0.943 | \n
Pseudo-second-order kinetic parameters for HA sorption and photocatalysis.
Catalyst | \nParameters | \nValue | \n
---|---|---|
\n | HA concentration (50 mg·L−1) | \n|
PAC-TiO2 | \nqe(mg*g−1) | \n9.95 | \n
k1(min−1) | \n0.0073 | \n|
R2 | \n0.955 | \n|
GAC-TiO2 | \nqe(mg*g−1) | \n1.64 | \n
k1(min−1) | \n0.0494 | \n|
R2 | \n0.913 | \n|
Z-TiO2 | \nqe(mg*g−1) | \n2.92 | \n
k1(min−1) | \n0.0142 | \n|
R2 | \n0.943 | \n|
\n | HA concentration (25 mg·L−1) | \n|
CNT-TiO2-Epoxy | \nqe(mg*g−1) | \n0.33 | \n
k1(min−1) | \n0.085 | \n|
R2 | \n0.995 | \n|
CNF-TiO2-Epoxy | \nqe(mg*g−1) | \n1.66 | \n
k1(min−1) | \n0.0019 | \n|
R2 | \n0.956 | \n
Pseudo-first-order kinetic parameters for HA photocatalysis.
Based on the results presented in Table 1, it can be seen that the PAC-TiO2 exhibited higher sorption capacity and the best kinetics for HA removal and the GAC-TiO2 exhibited the best photocatalytic kinetics, which are in accordance with the efficiency results. The worse results were achieved for TiO2 composite materials, which can be explained by the presence of epoxy matrix that reduced the active sites for the sorption and the photocatalysis. Also, the main difference was found between CNT-TiO2-Epoxy and CNF-TiO2-Epoxy due to the morphology and sizes of the nanostructured carbon component, better for CNT in comparison with CNF. For these types of material, the photocatalytic activity was better also for CNT-TiO2-Epoxy.
\nArsenic is a common contaminant in drinking water supplies especially for groundwater sources. Inorganic arsenic speciation in water consists of arsenite (AsIII) and arsenate (AsV), but As(III) is more problematic because of its high toxicity and the difficulty to be removed from water [29]. The comparative results regarding As(III) removal in the presence of HA showed a good efficiency for both sorption and photocatalysis using supported TiO2 material (Figure 11).
\nTime evolution of As(III) concentration during sorption and photocatalysis using PAC-TiO2 and GAC-TiO2.
Another common problem of groundwater source used for drinking water supply is given by the presence of ammonium, nitrite, and nitrate. Nitrate could not be removed from water on these tested materials, while ammonium and nitrate were removed from Z-TiO2 (Figure 12).
\nTime evolution of NO2− concentration during photolysis (a), photocatalysis using Z-TiO2 (b), of NH4+ concentration during photocatalysis using Z-TiO2 (c), and natural zeolite (d).
The results showed that ammonium is removed by sorption on the zeolite based on ionic exchange, which is proven by comparison with natural zeolite, while the nitrite removal is based on its oxidation process during UV irradiation, which is enhanced by the presence of the Z-TiO2 photocatalyst.
\nSince activated carbon is a versatile sorbent class for the retention of a wide spectrum of organic compounds and arsenic(III) and the zeolite exhibited an adsorption/ion-exchange capacity for ammonium, nitrite, and heavy metals, their common presence as mixed materials broadens the spectrum of contaminants that can be removed from the water.
\nIn this chapter, two types of composites obtained by two different methods and applied in the drinking water treatment were studied:
TiO2 supported on powdered activated carbon (PAC-TiO2), granular activated carbon (GAC-TiO2), and zeolite (Z-TiO2), namely, supported TiO2, obtained through sol-gel method.
TiO2 and multiwall carbon nanotubes and carbon nanofibers dispersed within epoxy matrix (CNT-TiO2-Epoxy, CNF-TiO2-Epoxy), namely, TiO2 composite, obtained through the two-roll mill method.
The sorption and photocatalysis studies showed that for HA removal, the sorption capacity of tested materials increased in order, PAC-TiO2 > Z-TiO2 > GAC-TiO2 > CNT-TiO2-Epoxy>CNF-TiO2-Epoxy, and for the photocatalytic activity, GAC-TiO2 > Z-TiO2 > PAC-TiO2 > CNT-TiO2-Epoxy> CNF-TiO2-Epoxy.
\nThe removal of pollutants/impurities dissolved in water is based, on the one hand, on the sorption capacity of activated carbon and/or zeolite, which exhibited selectivity for certain impurities dissolved under the lamp-off conditions. On the other hand, but taking into account the sorption phase, by starting the lamp, TiO2 on the active carbon surface and the zeolite acted by photocatalytic activity generating oxidation and reduction processes that cause the degradation and mineralization of the dissolved organic compounds and the transformation of the inorganic contaminants into the compounds that can be retained on the surface material or compounds that do not affect the quality of the water. Also, the oxidation and reduction processes under irradiation conditions allow the destruction of the contaminants and, implicitly, the cleaning of the sorbent surface. A mixture of zeolite and activated carbon as support for TiO2 could exhibit bifunctionality, depending on the water features. Thus, for low loading of water with contaminants that can be adsorbed on the filter material, the lamp is not switched on during system operation but only in the washing/regeneration stage, and for a water loaded with contaminants that cannot be adsorbed on the filter material, the system works with the lamp on, ensuring water decontamination and self-cleaning during operation.
\nThis work was supported by the Romanian National Research Programs PN-III-P2-2.1-PED-2016, PED 69/2017.
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