Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles
Identifieur interne : 000017 ( Pmc/Corpus ); précédent : 000016; suivant : 000018Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles
Auteurs : Eman AlzahraniSource :
- International Journal of Analytical Chemistry [ 1687-8760 ] ; 2015.
Abstract
The purification of industrial wastewater from dyes is becoming increasingly important since they are toxic or carcinogenic to human beings. Nanomaterials have been receiving significant attention due to their unique physical and chemical properties compared with their larger-size counterparts. The aim of the present investigation was to fabricate magnetic nanoparticles (MNPs) using a coprecipitation method, followed by coating with silver (Ag) in order to enhance the photocatalytic activity of the MNPs by loading metal onto them. The fabricated magnetic nanoparticles coated with Ag were characterised using different instruments such as a scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDAX) spectroscopy, and X-ray diffraction (XRD) analysis. The average size of the magnetic nanoparticles had a mean diameter of about 48 nm, and the average particle size changed to 55 nm after doping. The fabricated Ag-doped magnetic nanoparticles were used for the degradation of eosin Y under UV-lamp irradiation. The experimental results revealed that the use of fabricated magnetic nanoparticles coated with Ag can be considered as reliable methods for the removal of eosin Y since the slope of evaluation of pseudo-first-order rate constant from the slope of the plot between ln(
Url:
DOI: 10.1155/2015/797606
PubMed: 26617638
PubMed Central: 4649070
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles</title><author><name sortKey="Alzahrani, Eman" sort="Alzahrani, Eman" uniqKey="Alzahrani E" first="Eman" last="Alzahrani">Eman Alzahrani</name><affiliation><nlm:aff id="I1">Chemistry Department, Faculty of Science, Taif University, P.O. Box 888, Taif, Saudi Arabia</nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">26617638</idno><idno type="pmc">4649070</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC4649070</idno><idno type="RBID">PMC:4649070</idno><idno type="doi">10.1155/2015/797606</idno><date when="2015">2015</date><idno type="wicri:Area/Pmc/Corpus">000017</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">000017</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles</title><author><name sortKey="Alzahrani, Eman" sort="Alzahrani, Eman" uniqKey="Alzahrani E" first="Eman" last="Alzahrani">Eman Alzahrani</name><affiliation><nlm:aff id="I1">Chemistry Department, Faculty of Science, Taif University, P.O. Box 888, Taif, Saudi Arabia</nlm:aff></affiliation></author></analytic><series><title level="j">International Journal of Analytical Chemistry</title><idno type="ISSN">1687-8760</idno><idno type="eISSN">1687-8779</idno><imprint><date when="2015">2015</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>The purification of industrial wastewater from dyes is becoming increasingly important since they are toxic or carcinogenic to human beings. Nanomaterials have been receiving significant attention due to their unique physical and chemical properties compared with their larger-size counterparts. The aim of the present investigation was to fabricate magnetic nanoparticles (MNPs) using a coprecipitation method, followed by coating with silver (Ag) in order to enhance the photocatalytic activity of the MNPs by loading metal onto them. The fabricated magnetic nanoparticles coated with Ag were characterised using different instruments such as a scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDAX) spectroscopy, and X-ray diffraction (XRD) analysis. The average size of the magnetic nanoparticles had a mean diameter of about 48 nm, and the average particle size changed to 55 nm after doping. The fabricated Ag-doped magnetic nanoparticles were used for the degradation of eosin Y under UV-lamp irradiation. The experimental results revealed that the use of fabricated magnetic nanoparticles coated with Ag can be considered as reliable methods for the removal of eosin Y since the slope of evaluation of pseudo-first-order rate constant from the slope of the plot between ln(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) and the irradiation time was found to be linear. Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles would be considered an efficient photocatalyst to degrade textile dyes avoiding the tedious filtration step.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct><analytic><author><name sortKey="Gurr, E" uniqKey="Gurr E">E. Gurr</name></author></analytic></biblStruct><biblStruct><analytic><author><name sortKey="Shahid Ul Islam" uniqKey="Shahid Ul Islam">Shahid-ul-Islam</name></author><author><name sortKey="Mohammad, F" uniqKey="Mohammad F">F. Mohammad</name></author></analytic></biblStruct><biblStruct><analytic><author><name sortKey="Namasivayam, C" uniqKey="Namasivayam C">C. Namasivayam</name></author><author><name sortKey="Kavitha, D" uniqKey="Kavitha D">D. Kavitha</name></author></analytic></biblStruct><biblStruct><analytic><author><name sortKey="Gong, R" uniqKey="Gong R">R. Gong</name></author><author><name sortKey="Sun, Y" uniqKey="Sun Y">Y. Sun</name></author><author><name sortKey="Chen, J" uniqKey="Chen J">J. 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<front><journal-meta><journal-id journal-id-type="nlm-ta">Int J Anal Chem</journal-id><journal-id journal-id-type="iso-abbrev">Int J Anal Chem</journal-id><journal-id journal-id-type="publisher-id">IJAC</journal-id><journal-title-group><journal-title>International Journal of Analytical Chemistry</journal-title></journal-title-group><issn pub-type="ppub">1687-8760</issn><issn pub-type="epub">1687-8779</issn><publisher><publisher-name>Hindawi Publishing Corporation</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">26617638</article-id><article-id pub-id-type="pmc">4649070</article-id><article-id pub-id-type="doi">10.1155/2015/797606</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Article</subject></subj-group></article-categories><title-group><article-title>Photodegradation of Eosin Y Using Silver-Doped Magnetic Nanoparticles</article-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Alzahrani</surname><given-names>Eman</given-names></name><xref ref-type="aff" rid="I1"></xref><xref ref-type="corresp" rid="cor1"><sup>*</sup></xref></contrib></contrib-group><aff id="I1">Chemistry Department, Faculty of Science, Taif University, P.O. Box 888, Taif, Saudi Arabia</aff><author-notes><corresp id="cor1">*Eman Alzahrani: <email>em-s-z@hotmail.com</email></corresp><fn fn-type="other"><p>Academic Editor: Lawrence A. Bottomley</p></fn></author-notes><pub-date pub-type="ppub"><year>2015</year></pub-date><pub-date pub-type="epub"><day>4</day><month>11</month><year>2015</year></pub-date><volume>2015</volume><elocation-id>797606</elocation-id><history><date date-type="received"><day>21</day><month>8</month><year>2015</year></date><date date-type="accepted"><day>8</day><month>10</month><year>2015</year></date></history><permissions><copyright-statement>Copyright © 2015 Eman Alzahrani.</copyright-statement><copyright-year>2015</copyright-year><license license-type="open-access"><license-p>This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.</license-p></license></permissions><abstract><p>The purification of industrial wastewater from dyes is becoming increasingly important since they are toxic or carcinogenic to human beings. Nanomaterials have been receiving significant attention due to their unique physical and chemical properties compared with their larger-size counterparts. The aim of the present investigation was to fabricate magnetic nanoparticles (MNPs) using a coprecipitation method, followed by coating with silver (Ag) in order to enhance the photocatalytic activity of the MNPs by loading metal onto them. The fabricated magnetic nanoparticles coated with Ag were characterised using different instruments such as a scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDAX) spectroscopy, and X-ray diffraction (XRD) analysis. The average size of the magnetic nanoparticles had a mean diameter of about 48 nm, and the average particle size changed to 55 nm after doping. The fabricated Ag-doped magnetic nanoparticles were used for the degradation of eosin Y under UV-lamp irradiation. The experimental results revealed that the use of fabricated magnetic nanoparticles coated with Ag can be considered as reliable methods for the removal of eosin Y since the slope of evaluation of pseudo-first-order rate constant from the slope of the plot between ln(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) and the irradiation time was found to be linear. Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles would be considered an efficient photocatalyst to degrade textile dyes avoiding the tedious filtration step.</p></abstract></article-meta></front><body><sec id="sec1"><title>1. Introduction</title><p>In recent decades, environmental problems have attracted increasing attention all over the world. One type of environmental pollutants of concern is synthetic dyes, which are commonly used for colouring materials such as textiles, leather, paper, wool, printed matter, and cosmetics [<xref rid="B24" ref-type="bibr">1</xref>, <xref rid="B42" ref-type="bibr">2</xref>]. Although the exact number of the produced dyes in the world is not known, it is estimated that there are more than 100,000 different available dyes. These dyes are difficult to decolourise because of their complex aromatic structure, which originates from coal-tar-based hydrocarbons such as benzene, naphthalene, anthracene, toluene, and xylene [<xref rid="B45" ref-type="bibr">3</xref>–<xref rid="B58" ref-type="bibr">8</xref>]. Commonly, these dyes are discharged into the environment in the form of coloured wastewater by many industries without any prior treatment; however, many of them are known to be toxic or carcinogenic to human beings [<xref rid="B29" ref-type="bibr">9</xref>–<xref rid="B47" ref-type="bibr">11</xref>]. Therefore, several researchers are working on methods for the removal of dyes from wastewater before their discharge into downstream bodies of water [<xref rid="B15" ref-type="bibr">12</xref>–<xref rid="B39" ref-type="bibr">16</xref>].</p><p>There are several methods that have been utilised for the removal of dyes from industrial wastewater, for example, adsorption, nanofiltration, ozonation, and electroflotation [<xref rid="B55" ref-type="bibr">17</xref>–<xref rid="B19" ref-type="bibr">19</xref>]. All of these processes have different capabilities for removing dyes. Among these methods, adsorption has been found to be the best technique for wastewater purification [<xref rid="B8" ref-type="bibr">20</xref>–<xref rid="B50" ref-type="bibr">22</xref>], due to the simplicity of the procedure, ease of operation, and its nonsensitivity to toxic substances. The purification of wastewater from harmful dyes can be performed using activated carbon, which has a high surface area [<xref rid="B36" ref-type="bibr">23</xref>–<xref rid="B2" ref-type="bibr">26</xref>]; however, it also has a high waste cost. Other materials that can be utilised are alum, ferric salt, or lime. Although the cost of these materials is cheap, they suffer from several severe drawbacks [<xref rid="B14" ref-type="bibr">27</xref>–<xref rid="B11" ref-type="bibr">30</xref>].</p><p>The field of nanotechnology is one of the most active areas of research in modern materials science. The application of nanoscale materials, which range from 1 to 100 nm, is a key emerging area of nanotechnology. There is an increased demand for nanoparticles because of their wide applicability in various areas, for example, electronics, catalysis, chemistry, energy, and medicine [<xref rid="B78" ref-type="bibr">31</xref>–<xref rid="B5" ref-type="bibr">34</xref>].</p><p>Magnetic nanoparticles (MNPs) are a type of nanoparticles that can be manipulated using a magnetic field. MNPs are attracting significant attention due to their large surface area, high magnetic properties, high thermal stability, high mechanical strength, and lack of toxicity [<xref rid="B71" ref-type="bibr">35</xref>–<xref rid="B35" ref-type="bibr">37</xref>]. Moreover, MNPs can be rapidly prepared, have high separation efficiency, are cost-effective, and provide for a simple operational process. They are utilised in applications such as magnetic drug targeting, magnetic resonance imaging for clinical diagnosis, recording material, and biomedical applications [<xref rid="B62" ref-type="bibr">38</xref>–<xref rid="B6" ref-type="bibr">41</xref>].</p><p>MNPs possessing magnetite (Fe<sub>3</sub>O<sub>4</sub>) or maghemite (<italic>γ</italic>-Fe<sub>2</sub>O<sub>3</sub>) core chemistry have been used to solve a range of environmental problems; for example, MNPs have been utilised for the purification of wastewater by removing heavy metals, alkalinity, and hardness, as well as natural organic compounds and salt. This is due to their simple fabrication, easy optimisation of their size and morphology, and fast magnetic separation under an external magnetic field [<xref rid="B75" ref-type="bibr">42</xref>–<xref rid="B70" ref-type="bibr">45</xref>].</p><p>Iron oxide nanoparticles can be fabricated using different methods, for example, coprecipitation, energy milling, reduction, and ultrasonic-assisted impregnation. The coprecipitation method is based on mixing ferrous and ferric ions in the ratio of 1 to 2 in an alkaline medium. The main advantage of this method is that it produces fine and stoichiometric particles of single and multicomponent metal oxides [<xref rid="B72" ref-type="bibr">46</xref>–<xref rid="B51" ref-type="bibr">50</xref>].</p><p>In order to improve the physicochemical properties of MNPs and to achieve different kinds of applications, modification of the surfaces of MNPs with functional groups is necessary [<xref rid="B73" ref-type="bibr">51</xref>, <xref rid="B38" ref-type="bibr">52</xref>]. The doping of MNPs with metals can resolve the problem of the fast recombination of charge carriers, which happens within nanoseconds, by trapping and subsequently transferring the photoexcited electrons onto the surface of photocatalyst, resulting in decreased recombination of the electron-hole pairs [<xref rid="B57" ref-type="bibr">53</xref>, <xref rid="B27" ref-type="bibr">54</xref>].</p><p>According to our literature survey, only very few studies have been carried out on the use of MNPs doping with metal for the photodegradation of harmful dyes. Therefore, the purpose of the present paper is to describe the fabrication of magnetic nanoparticles (MNPs) using the precipitation method, followed by doping of the MNPs with Ag. Characterisations of the fabricated Ag-doped magnetic nanoparticles were performed by studying the physical properties of the fabricated nanoparticles using scanning electron microscopy (SEM) analysis, transmission electron microscopy (TEM) analysis, energy-dispersive X-ray analysis (EDAX), and X-ray diffraction (XRD) analysis. The fabricated materials were used for the photodegradation of a model dye, namely, eosin Y (the characteristics of eosin Y are given in <xref ref-type="table" rid="tab1">Table 1</xref>), in the presence of ultraviolet light (UV). Furthermore, the photocatalytic activity of the Ag-MNPs was compared with naked MNPs. Moreover, the degradation kinetics were followed to study the photocatalytic efficiency of the Ag-MNPs.</p></sec><sec id="sec2"><title>2. Experimental</title><sec id="sec2.1"><title>2.1. Chemicals and Materials</title><p>Iron(II) sulfate heptahydrate (FeSO<sub>4</sub>·7H<sub>2</sub>O, 98%), Mwt. = 151.91 g mol<sup>−1</sup>, sodium nitrite (NaNO<sub>3</sub>, 99%), and eosin Y were purchased from Sigma-Aldrich (Nottingham, UK). Sodium hydroxide (NaOH) was purchased from Loba Chemie Pvt. Ltd. (Mumbai, India). Silver nitrate (AgNO<sub>3</sub>, 99.85%) and sodium carbonate (Na<sub>2</sub>CO<sub>3</sub>) were purchased from Acros Organics (Loughborough, UK). Cylindrical rod magnets (40 mm diameter × 40 mm thickness) for settlement of the magnetic nanoparticles were purchased from Magnet Expert Ltd. (Tuxford, UK). Distilled water was employed for preparing all the solutions and reagents.</p></sec><sec id="sec2.2"><title>2.2. Instrumentation</title><p>The magnetic stirrer and heater were purchased from Fisher Scientific Co. Ltd. (Shanghai, China). The oven was from Memmert (Nuremberg, Germany). X-ray diffraction (XRD) patterns were obtained using a Bruker diffractometer D8-ADVANCE with CuK<sub><italic>α</italic>1</sub> radiation (Coventry, UK). The transmission electron microscope (TEM) came from JEOL Ltd. (Welwyn Garden City, UK). The scanning electron microscope (SEM) with unit energy-dispersive X-ray analysis (EDAX) was obtained from JEOL JSM 6390 LA Analytical (Tokyo, Japan). The UV lamp (<italic>λ</italic> = 365 nm) was purchased from Spectronic Analytical Instruments (Leeds, UK). The UV-Vis spectrophotometer was from Thermo Scientific GENESYS 10S (Toronto, Canada).</p></sec><sec id="sec2.3"><title>2.3. Preparation of the Magnetic Iron Oxide Nanoparticles</title><p>Magnetic nanoparticles (MNPs) were prepared as described by Tan and Bakar [<xref rid="B66" ref-type="bibr">55</xref>], with some modification. MNPs were obtained by dissolving 3.3 g of FeSO<sub>4</sub>·7H<sub>2</sub>O and 2 g of NaNO<sub>3</sub> in 50 mL of distilled water. Then, 20 mL of NaOH solution (2.5 M) was added to the mixture while it was heated up to 80°C. The reaction was allowed to proceed at 80°C under constant stirring to ensure the complete growth of the nanoparticle crystals. After 30 minutes, the resulting suspension was cooled down to room temperature and washed with distilled water repeatedly to remove unreacted chemicals. The Fe<sub>3</sub>O<sub>4</sub> magnetic nanoparticles were separated using an external magnet and dried in an oven at 50°C overnight before the coating.</p></sec><sec id="sec2.4"><title>2.4. Doping of MNPs with Ag</title><p>The prepared magnetic nanoparticles were doped with Ag. This was performed by mixing 10 g of magnetic nanoparticles with 10 mL of silver nitrate solution (0.1 M). Then, 10 mL of sodium carbonate (1%) solution was added. The suspension was dried at 80°C for 24 h, and finally the formed powder was calcinated at 400°C for 6 h in a furnace. The formed Ag-doped MNPs were washed with distilled water. The product was dried at room temperature for 12 h in a vacuum desiccator.</p></sec><sec id="sec2.5"><title>2.5. Characterisation of the Prepared Materials</title><p>The morphology and mean size of the samples were determined by transmission electron microscopy (TEM). A drop of well-dispersed nanoparticle dispersion was placed onto the amorphous carbon-coated 200-mesh copper grid and allowed to dry at ambient temperature, and then the grid was scanned. The average size of about 100 nanoparticles of each sample was measured from the TEM images by using the ImageJ software. The morphology of the fabricated magnetic nanoparticles before and after doping with Ag was characterised by SEM analysis. The compositional analysis was performed using energy-dispersive X-ray analysis (EDAX). Phase identification and structural analysis of the magnetic nanoparticles were carried out using X-ray diffraction (XRD) with the CuK<sub><italic>α</italic></sub> radiation in the 2-theta range from 20° to 70°.</p></sec><sec id="sec2.6"><title>2.6. Photocatalytic Degradation of Eosin Y</title><p>The photocatalytic activity of Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles was investigated by the decolourisation of eosin Y in aqueous solution. All the degradation reactions were performed according to the following procedure: 50 mg of photocatalyst was added to 100 mL of aqueous dye solution (4 × 10<sup>−4</sup> M) placed in a cylindrical glass vessel. Before exposure to the UV lamp, the suspension was magnetically stirred at 600 rpm for 1 h in the dark in order to achieve the adsorption-desorption equilibrium between the photocatalyst and the dye. The reaction was performed with constant magnetic stirring during the reaction. A 2 mL aliquot was withdrawn from the mixture solution at 60 min intervals. The degradation of eosin Y was spectrometrically monitored with a UV-Vis spectrophotometer at a wavelength between 350 and 800 nm according to the dye. The photocatalyst was precipitated from the solution by applying an external magnet and then washed with distilled water and stored for further use. The efficiency of the photocatalytic degradation of the fabricated materials was calculated based on the degree of absorption in the absorption spectra of the dye solution with respect to the intensity corresponding to <italic>λ</italic><sub>max</sub> of eosin Y (515 nm) by using the equation given below [<xref rid="B16" ref-type="bibr">56</xref>–<xref rid="B3" ref-type="bibr">58</xref>]:<disp-formula id="eq1"><label>(1)</label><mml:math id="M1"><mml:mtable style="T1"><mml:mtr><mml:mtd><mml:mi>D</mml:mi><mml:mi>%</mml:mi><mml:mo>=</mml:mo><mml:mfrac><mml:mrow><mml:msub><mml:mrow><mml:mi>C</mml:mi></mml:mrow><mml:mrow><mml:mi>o</mml:mi></mml:mrow></mml:msub><mml:mo>−</mml:mo><mml:mi>C</mml:mi></mml:mrow><mml:mrow><mml:msub><mml:mrow><mml:mi>C</mml:mi></mml:mrow><mml:mrow><mml:mi>o</mml:mi></mml:mrow></mml:msub></mml:mrow></mml:mfrac><mml:mo>×</mml:mo><mml:mn mathvariant="normal">100</mml:mn><mml:mo>=</mml:mo><mml:mfrac><mml:mrow><mml:msub><mml:mrow><mml:mi>A</mml:mi></mml:mrow><mml:mrow><mml:mi>o</mml:mi></mml:mrow></mml:msub><mml:mo>−</mml:mo><mml:mi>A</mml:mi></mml:mrow><mml:mrow><mml:msub><mml:mrow><mml:mi>A</mml:mi></mml:mrow><mml:mrow><mml:mi>o</mml:mi></mml:mrow></mml:msub></mml:mrow></mml:mfrac><mml:mo>×</mml:mo><mml:mn mathvariant="normal">100</mml:mn><mml:mo>,</mml:mo></mml:mtd></mml:mtr></mml:mtable></mml:math></disp-formula>where <italic>C</italic><sub><italic>o</italic></sub> is the initial concentration of the dye and <italic>C</italic> is the concentration of the dye after irradiation in a selected time interval. Parameters <italic>A</italic><sub><italic>o</italic></sub> and <italic>A</italic> are the absorbance of eosin Y solutions in the 515 nm wavelength at the initial and at any time thereafter, respectively.</p></sec></sec><sec id="sec3"><title>3. Results and Discussion </title><sec id="sec3.1"><title>3.1. Preparation of Fe<sub>3</sub>O<sub>4</sub> and the Ag-Doped Fe<sub>3</sub>O<sub>4</sub> Nanoparticles</title><p>In this study, magnetic nanoparticles (MNPs) were fabricated. The reason for choosing this type of nanoparticle was because it is easy to fabricate and it is easy to separate it from the solution by using an external magnet [<xref rid="B62" ref-type="bibr">38</xref>, <xref rid="B10" ref-type="bibr">59</xref>, <xref rid="B53" ref-type="bibr">60</xref>]. The chemical precipitation technique was used to prepare the magnetic nanoparticles. This technique is probably the most common and efficient method to obtain magnetic particles [<xref rid="B4" ref-type="bibr">40</xref>, <xref rid="B41" ref-type="bibr">61</xref>, <xref rid="B48" ref-type="bibr">62</xref>]. The fabrication of MNPs was performed by mixing iron(II) sulfate heptahydrate and sodium nitrite in purified water. Complete precipitation of Fe<sub>3</sub>O<sub>4</sub> nanoparticles was achieved under alkaline condition, which was 20 mL of NaOH solution (2.5 M). When NaOH solution was added to the FeSO<sub>4</sub>, Fe(OH)<sub>2</sub> was initially formed, which was then oxidised to the Fe<sub>3</sub>O<sub>4</sub> nanoparticle [<xref rid="B41" ref-type="bibr">61</xref>, <xref rid="B79" ref-type="bibr">63</xref>, <xref rid="B40" ref-type="bibr">64</xref>]. Finally, the formed magnetic nanoparticles were separated from the reaction medium by a permanent magnet field and washed with distilled water to remove excess ions such as SO<sub>4</sub><sup>2−</sup> and NO<sub>3</sub><sup>−</sup>.</p><p>The MNPs were doped with Ag in order to obtain a higher photocatalytic efficiency than the naked Fe<sub>3</sub>O<sub>4</sub> nanoparticles. After calcination, the colour of the Fe<sub>3</sub>O<sub>4</sub> nanoparticles turned from black to brownish. <xref ref-type="fig" rid="fig1"> Figure 1</xref> shows photographs of aqueous solutions of the unsupported Fe<sub>3</sub>O<sub>4</sub> nanoparticles (a) and Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles (b) in vials before and after magnetic separation using an external magnetic field, while <xref ref-type="fig" rid="fig1">Figure 1(c)</xref> shows the dried fabricated materials.</p></sec><sec id="sec3.2"><title>3.2. Characterisation of the Fabricated Materials</title><p>The catalytic power of the photocatalysts is affected by the size of the nanoparticles, the distribution of the sizes, and the morphology, since the size of nanoparticles has a strong effect on the energy levels of the photocatalysts [<xref rid="B74" ref-type="bibr">65</xref>–<xref rid="B1" ref-type="bibr">67</xref>]. Therefore, to obtain a good understanding of the photocatalytic processes, the size of the particles and the morphology should be studied. The fabricated materials were thus characterised using different techniques, namely, TEM analysis and SEM analysis. In addition, compositional analysis was performed using energy-dispersive X-ray analysis (EDAX). For phase identification and the structural analysis of the magnetic nanoparticles, an X-ray diffraction (XRD) instrument was utilised.</p><sec id="sec3.2.1"><title>3.2.1. TEM Analysis</title><p>A transmission electron microscope is a good tool for extraction of the size and shape data because it yields real images from which measurements can be made [<xref rid="B5" ref-type="bibr">34</xref>, <xref rid="B52" ref-type="bibr">68</xref>, <xref rid="B46" ref-type="bibr">69</xref>]; therefore, this was used in order to recognise the morphology and the size of the prepared materials. <xref ref-type="fig" rid="fig2"> Figure 2</xref> shows TEM micrographs of the unsupported Fe<sub>3</sub>O<sub>4</sub> nanoparticles and the Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles using different magnifications. Although the fabricated magnetic nanoparticles were crystalline and tended to have identifiable shapes (rectangles and squares), there were some differences in the comparison. The TEM images showed that the magnetic nanoparticles appeared darker after coating with Ag and they seemed more compact compared with Fe<sub>3</sub>O<sub>4</sub> nanoparticles, indicating that Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles had a higher density than that of Fe<sub>3</sub>O<sub>4</sub> nanoparticles. The particle size distribution histograms for MNPs and Ag-MNPs have been determined from TEM images (<xref ref-type="fig" rid="fig2">Figure 2</xref>), and the corresponding size distribution histograms are shown in <xref ref-type="fig" rid="fig3">Figure 3</xref>. The average size of the MNPs was 48 nm within size ranging from 24 to 60 nm. The size distribution of Ag-MNPs ranged from 30 nm to 62 nm, within average size of 55 nm. Commonly, the average diameter of coating MNPs will increase in the range of 0–5 nm compared with the naked MNPs [<xref rid="B73" ref-type="bibr">51</xref>]. It was found that the TEM analysis served as an important technique for providing evidence of the formation of the Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles.</p></sec><sec id="sec3.2.2"><title>3.2.2. SEM-EDAX Analysis</title><p>The morphology and structures of the Fe<sub>3</sub>O<sub>4</sub> nanoparticles and the Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles were also investigated by SEM analysis. <xref ref-type="fig" rid="fig4"> Figure 4</xref> shows the SEM micrographs of the Fe<sub>3</sub>O<sub>4</sub> nanoparticles and the Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles in different magnifications, which suggest that the prepared magnetic nanoparticles have an irregular crystalline form, and furthermore, the surface morphology analysis demonstrates the agglomeration of many ultrafine particles. In addition, no significant morphological differences could be observed between the Fe<sub>3</sub>O<sub>4</sub> nanoparticles and the Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles.</p><p>In order to further identify the chemical composition of the fabricated materials, EDAX was utilised to recognise the distribution of Fe, O, and Ag atoms in the prepared materials. The characterisations of the fabricated Fe<sub>3</sub>O<sub>4</sub> nanoparticles and Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles using EDAX are shown in <xref ref-type="fig" rid="fig5">Figure 5</xref>. The EDAX spectra showed strong peaks of Fe and O. It was observed that there was a new peak in the Ag-doped Fe<sub>3</sub>O<sub>4</sub> sample, representing Ag, which confirms the doping of the magnetic nanoparticles with silver.</p></sec><sec id="sec3.2.3"><title>3.2.3. XRD Analysis</title><p>The obtained samples were analysed by X-ray diffraction (XRD) using a diffractometer with high-intensity CuK<sub><italic>α</italic></sub> radiation (<italic>λ</italic> = 1.54065 Å) and measured from 10° to 70°, and the results are depicted in <xref ref-type="fig" rid="fig6">Figure 6</xref>. For the Fe<sub>3</sub>O<sub>4</sub> diffraction peaks, seven characteristic peaks at 30°, 35°, 37°, 43°, 53°, 57°, and 62° were seen, corresponding to the (220), (311), (222), (400), (422), (511), and (440) crystal planes of pure Fe<sub>3</sub>O<sub>4</sub> with a cubic spinel structure of the magnetite [<xref rid="B79" ref-type="bibr">63</xref>, <xref rid="B18" ref-type="bibr">70</xref>, <xref rid="B13" ref-type="bibr">71</xref>]. No characteristic peaks of impurities were detected in the XRD pattern, indicating the high purity of fabricated materials. The XRD patterns of Ag-doped Fe<sub>3</sub>O<sub>4</sub> did not show diffraction peaks due to the doping of Ag, since there was no peak of Ag observed; therefore, it is suggested that the silver dopant was merely placed on the surface of the crystals. The same results have been obtained by [<xref rid="B34" ref-type="bibr">72</xref>].</p></sec></sec><sec id="sec3.3"><title>3.3. Photodegradation of Eosin Y </title><sec id="sec3.3.1"><title>3.3.1. Comparison between the Naked MNPs and the Ag-MNPs Nanoparticles</title><p>An organic dye, namely, eosin Y, in aqueous solution was utilised in order to check the performance of the fabricated materials, and their performance was compared with naked magnetic nanoparticles. The photodegradation experiment was performed by adding 50 mg of catalyst to 100 mL of the dye solution (4 × 10<sup>−4</sup> M). The suspension was magnetically stirred at 600 rpm in the dark for 1 h in order to attain adsorption-desorption equilibrium before the irradiation by UV light (365 nm). The main advantage of using the UV light was to produce electron and hole pair (e<sup>−</sup>/h<sup>+</sup>) with high energy state that migrate to the nanoparticle surface and initiate a wide range of chemical reactions [<xref rid="B31" ref-type="bibr">73</xref>].</p><p>The suspension was magnetically stirred throughout the experiment. For different irradiation times (0–240 min), at every 60 min interval, an aliquot (2 mL) was taken out. It was observed that the intense orange colour of the initial solution disappears gradually and becomes colourless as the irradiation time increases, indicating the degradation of the dye under UV light irradiation, as can be seen in <xref ref-type="fig" rid="fig7">Figure 7</xref>.</p><p>The absorption spectra of the dye solution were recorded, as shown in <xref ref-type="fig" rid="fig8">Figure 8</xref>, which shows the UV-Vis time-dependent absorption spectrum during the photocatalytic reaction of eosin Y. From the figure, it can be seen that the absorption spectrum maximum of eosin Y steadily decreases as the exposure time of UV light increases from 0 to 240 min, indicating the process of photodecomposition of the dye.</p><p>The photocatalytic activities of the naked Fe<sub>3</sub>O<sub>4</sub> nanoparticles and a solution without the photocatalyst, for comparison, were also investigated. It was found that, without adding the photocatalyst, the degradation of eosin Y was very slow at only 5%, while the naked Fe<sub>3</sub>O<sub>4</sub> nanoparticles showed lower photocatalytic degradation of 40%. The colour removal process of eosin Y using Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles was significantly higher, reaching almost 90.12% decolourisation. <xref ref-type="fig" rid="fig9"> Figure 9</xref> shows the plot of <italic>C</italic>/<italic>C</italic><sub><italic>o</italic></sub> versus irradiation time. From studying the degradation of eosin Y, it was found that the UV light photocatalytic performance varies in the following order: without catalyst < naked Fe<sub>3</sub>O<sub>4</sub> nanoparticles < Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles.</p><p><xref ref-type="fig" rid="fig10">Figure 10</xref> represents the mechanism for the role of Ag coating in Fe<sub>3</sub>O<sub>4</sub> nanoparticles. During the photocatalytic reaction, there will be promotion of an electron from the valence band to the conduction band; thus electron-hole (e<sup>−</sup>/h<sup>+</sup>) pairs will form. The electron in the conduction band is removed by reaction with oxygen dissolved in water while the hole in the valence band can react with water or OH<sup>−</sup> that are absorbed on the surface of the silver-doped MNPs in order to give hydroxyl radical (<sup>•</sup>OH), which is utilised as a powerful oxidizing agent in order to convert organic pollutants into CO<sub>2</sub>, H<sub>2</sub>O, and less toxic by-products of low molecular weight [<xref rid="B31" ref-type="bibr">73</xref>]. The better photocatalytic activity shown by Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles over naked Fe<sub>3</sub>O<sub>4</sub> nanoparticles can be explained on the basis of silver being acceptor impurity in doping of Fe<sub>3</sub>O<sub>4</sub>. Ag acts as an electron trap and prevents the electron hole recombination that is an important factor in determining the photocatalytic activity [<xref rid="B34" ref-type="bibr">72</xref>, <xref rid="B44" ref-type="bibr">74</xref>].</p></sec><sec id="sec3.3.2"><title>3.3.2. Kinetic Analysis</title><p>The rate of reaction in the photodegradation experiment was calculated using pseudo-first-order kinetics: In(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) = <italic>kt</italic>, where <italic>C</italic><sub><italic>o</italic></sub> and <italic>C</italic> are the absorption measured at different illumination times, <italic>k</italic> is the reaction rate, and <italic>t</italic> is the reaction time during the decomposition of eosin Y [<xref rid="B9" ref-type="bibr">75</xref>–<xref rid="B77" ref-type="bibr">79</xref>]. The reaction rate (<italic>k</italic>) for the photodecomposition of eosin Y was calculated by drawing a graph between In(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) and <italic>t</italic>. <xref ref-type="fig" rid="fig11"> Figure 11</xref> presents the relationship between In(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) and <italic>t</italic> as a function of irradiation time in the presence of Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles. The figure shows that the photocatalytic degradation follows perfectly the pseudo-first-order kinetics, and the fairness of the fit is indicated by the linear regression value, <italic>R</italic><sup>2</sup> = 0.9938.</p></sec><sec id="sec3.3.3"><title>3.3.3. Reuse of the Photocatalyst</title><p>The reuse and the stability of Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles were studied in order to see the cost-effectiveness of the method. This was performed in a very simple way. After the degradation of eosin Y, the Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles were separated easily from the solution using a magnet, while the supernatant was decanted. Then, the magnetic nanoparticles were washed with distilled water and reused for degradation with a fresh lot of eosin Y solution. As can be seen in <xref ref-type="fig" rid="fig12">Figure 12</xref>, after using the Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles for three times, the photodegradation of eosin Y did not show any significant loss of activity. These results confirmed that the Ag-Fe<sub>3</sub>O<sub>4</sub> nanoparticles are not photocorroded during photocatalytic oxidation of the dye.</p></sec></sec></sec><sec id="sec4"><title>4. Conclusions</title><p>Photocatalysis has been ascertained to be a promising method for the removal of harmful dyes from industrial wastewater. In this study, the fabrication of MNPs with coating of Ag was successfully performed. The morphology of the fabricated magnetic nanoparticles before and after the modification with silver was characterised using TEM analysis to conduct the size investigations; SEM analysis was carried out for the surface morphology analysis and EDAX for the compositional analysis. The crystalline structures of the nanoparticles were identified with XRD, which showed the XRD patterns of the Fe<sub>3</sub>O<sub>4</sub>. The experimental results showed that the Ag-MNPs were more effective in enhancing the photocatalytic degradation of eosin Y over naked MNPs. Moreover, the fabricated materials were easily recovered by using an external magnet after the treatment of eosin Y. It is suggested that the UV/Ag-Fe<sub>3</sub>O<sub>4</sub> system could be used as a useful technique for the removal of harmful dyes from industrial wastewater. Work is currently investigating different azo dyes using the fabricated Ag-MNPs nanoparticles.</p></sec></body><back><ack><title>Acknowledgment </title><p>This work was funded by King Abdulaziz City for Science and Technology (KACST).</p></ack><sec sec-type="conflict"><title>Conflict of Interests</title><p>The author declares that there is no conflict of interests regarding the publication of this paper.</p></sec><ref-list><ref id="B24"><label>1</label><element-citation publication-type="book"><person-group person-group-type="author"><name><surname>Gurr</surname><given-names>E.</given-names></name></person-group><source><italic>Synthetic Dyes in Biology, Medicine and Chemistry</italic></source><year>2012</year><publisher-name>Elsevier</publisher-name></element-citation></ref><ref id="B42"><label>2</label><element-citation publication-type="journal"><person-group person-group-type="author"><name><surname>Shahid-ul-Islam</surname></name><name><surname>Mohammad</surname><given-names>F.</given-names></name></person-group><article-title>High-energy radiation induced sustainable coloration and functional finishing of textile materials</article-title><source><italic>Industrial & Engineering Chemistry Research</italic></source><year>2015</year><volume>54</volume><issue>15</issue><fpage>3727</fpage><lpage>3745</lpage><pub-id pub-id-type="doi">10.1021/acs.iecr.5b00524</pub-id></element-citation></ref><ref id="B45"><label>3</label><element-citation publication-type="journal"><person-group person-group-type="author"><name><surname>Namasivayam</surname><given-names>C.</given-names></name><name><surname>Kavitha</surname><given-names>D.</given-names></name></person-group><article-title>Removal of Congo Red from water by adsorption onto activated carbon prepared from coir pith, an agricultural solid waste</article-title><source><italic>Dyes and Pigments</italic></source><year>2002</year><volume>54</volume><issue>1</issue><fpage>47</fpage><lpage>58</lpage><pub-id pub-id-type="doi">10.1016/s0143-7208(02)00025-6</pub-id><pub-id pub-id-type="other">2-s2.0-0036638913</pub-id></element-citation></ref><ref id="B20"><label>4</label><element-citation publication-type="journal"><person-group person-group-type="author"><name><surname>Gong</surname><given-names>R.</given-names></name><name><surname>Sun</surname><given-names>Y.</given-names></name><name><surname>Chen</surname><given-names>J.</given-names></name><name><surname>Liu</surname><given-names>H.</given-names></name><name><surname>Yang</surname><given-names>C.</given-names></name></person-group><article-title>Effect of chemical modification on dye adsorption capacity of peanut hull</article-title><source><italic>Dyes and Pigments</italic></source><year>2005</year><volume>67</volume><issue>3</issue><fpage>175</fpage><lpage>181</lpage><pub-id pub-id-type="doi">10.1016/j.dyepig.2004.12.003</pub-id><pub-id pub-id-type="other">2-s2.0-15344338549</pub-id></element-citation></ref><ref id="B25"><label>5</label><element-citation publication-type="book"><person-group person-group-type="author"><name><surname>Hasan</surname><given-names>M. 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The size distribution was obtained by counting 100 nanoparticles for each sample.</p></caption><graphic xlink:href="IJAC2015-797606.003"></graphic></fig><fig id="fig4" orientation="portrait" position="float"><label>Figure 4</label><caption><p>SEM micrographs of Fe<sub>3</sub>O<sub>4</sub> nanoparticles ((a), (c)) and Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles ((b), (d)) at different magnifications.</p></caption><graphic xlink:href="IJAC2015-797606.004"></graphic></fig><fig id="fig5" orientation="portrait" position="float"><label>Figure 5</label><caption><p>EDAX of (a) Fe<sub>3</sub>O<sub>4</sub> nanoparticles and (b) Ag-doped Fe<sub>3</sub>O<sub>4</sub> nanoparticles.</p></caption><graphic xlink:href="IJAC2015-797606.005"></graphic></fig><fig id="fig6" orientation="portrait" position="float"><label>Figure 6</label><caption><p>XRD pattern of Fe<sub>3</sub>O<sub>4</sub> nanoparticles.</p></caption><graphic xlink:href="IJAC2015-797606.006"></graphic></fig><fig id="fig7" orientation="portrait" position="float"><label>Figure 7</label><caption><p>Photographs of eosin Y after treatment with the synthesised Ag-Fe<sub>3</sub>O<sub>4</sub> powder at different time intervals; the colour of eosin Y solution faded, indicating degradation of the dye.</p></caption><graphic xlink:href="IJAC2015-797606.007"></graphic></fig><fig id="fig8" orientation="portrait" position="float"><label>Figure 8</label><caption><p>UV-Vis absorption spectra of eosin Y during the course of reaction with the synthesised Ag-MNP powder at different time intervals under ultraviolet light irradiation at room temperature.</p></caption><graphic xlink:href="IJAC2015-797606.008"></graphic></fig><fig id="fig9" orientation="portrait" position="float"><label>Figure 9</label><caption><p>Photodegradation of eosin Y as a function of irradiation time in the absence and presence of MNPs or Ag-MNPs.</p></caption><graphic xlink:href="IJAC2015-797606.009"></graphic></fig><fig id="fig10" orientation="portrait" position="float"><label>Figure 10</label><caption><p>Schematic diagram of the reaction mechanism involved in photocatalytic activity of Ag-MNPs nanoparticles.</p></caption><graphic xlink:href="IJAC2015-797606.010"></graphic></fig><fig id="fig11" orientation="portrait" position="float"><label>Figure 11</label><caption><p>Plot of In(<italic>C</italic><sub><italic>o</italic></sub>/<italic>C</italic>) versus irradiation time.</p></caption><graphic xlink:href="IJAC2015-797606.011"></graphic></fig><fig id="fig12" orientation="portrait" position="float"><label>Figure 12</label><caption><p>Recycled photocatalytic degradation of eosin Y.</p></caption><graphic xlink:href="IJAC2015-797606.012"></graphic></fig><table-wrap id="tab1" orientation="portrait" position="float"><label>Table 1</label><caption><p>The characteristics of eosin Y dye.</p></caption><table frame="hsides" rules="groups"><tbody><tr><td align="left" rowspan="1" colspan="1">Chemical name</td><td align="center" rowspan="1" colspan="1">2-(2,4,5,7-Tetrabromo-6-oxido-3-oxo-3<italic>H</italic>-xanthen-9-yl)benzoate</td></tr><tr><td align="center" colspan="2" rowspan="1"><hr></hr></td></tr><tr><td align="left" rowspan="1" colspan="1">Chemical formula</td><td align="center" rowspan="1" colspan="1">C<sub>20</sub>H<sub>8</sub>Br<sub>4</sub>O<sub>5</sub></td></tr><tr><td align="center" colspan="2" rowspan="1"><hr></hr></td></tr><tr><td align="left" rowspan="1" colspan="1">Chemical structure</td><td align="center" rowspan="1" colspan="1"><inline-graphic xlink:href="IJAC2015-797606.tab1.i001.jpg"></inline-graphic></td></tr><tr><td align="center" colspan="2" rowspan="1"><hr></hr></td></tr><tr><td align="left" rowspan="1" colspan="1">Molecular weight</td><td align="center" rowspan="1" colspan="1">647.89 g mol<sup>−1</sup></td></tr><tr><td align="center" colspan="2" rowspan="1"><hr></hr></td></tr><tr><td align="left" rowspan="1" colspan="1">Type of dye</td><td align="center" rowspan="1" colspan="1">Anionic dye</td></tr><tr><td align="center" colspan="2" rowspan="1"><hr></hr></td></tr><tr><td align="left" rowspan="1" colspan="1"><italic>λ</italic><sub>max</sub></td><td align="center" rowspan="1" colspan="1">515 nm</td></tr></tbody></table></table-wrap></floats-group></pmc></record>Pour manipuler ce document sous Unix (Dilib)
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