<?xml version="1.0" encoding="UTF-8"?><!DOCTYPE article  PUBLIC "-//NLM//DTD Journal Publishing DTD v3.0 20080202//EN" "http://dtd.nlm.nih.gov/publishing/3.0/journalpublishing3.dtd"><article xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" dtd-version="3.0" xml:lang="en" article-type="research article"><front><journal-meta><journal-id journal-id-type="publisher-id">JMMCE</journal-id><journal-title-group><journal-title>Journal of Minerals and Materials Characterization and Engineering</journal-title></journal-title-group><issn pub-type="epub">2327-4077</issn><publisher><publisher-name>Scientific Research Publishing</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.4236/jmmce.2020.84013</article-id><article-id pub-id-type="publisher-id">JMMCE-100951</article-id><article-categories><subj-group subj-group-type="heading"><subject>Articles</subject></subj-group><subj-group subj-group-type="Discipline-v2"><subject>Chemistry&amp;Materials Science</subject><subject> Engineering</subject></subj-group></article-categories><title-group><article-title>
 
 
  Compositional, Structural, Surface Characterizations of Natural Magnetite from Air Massif (Niger) in Relation to Its Catalytic Activity
 
</article-title></title-group><contrib-group><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Mamane</surname><given-names>Souley Abdoul Aziz</given-names></name><xref ref-type="aff" rid="aff1"><sup>1</sup></xref><xref ref-type="corresp" rid="cor1"><sup>*</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Adouby</surname><given-names>Kopoin</given-names></name><xref ref-type="aff" rid="aff2"><sup>2</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>Ousmane</surname><given-names>Mahamane Sani</given-names></name><xref ref-type="aff" rid="aff3"><sup>3</sup></xref></contrib></contrib-group><aff id="aff1"><addr-line>Département d’Energie Fossile, Institut Universitaire de Technologie, Université d’Agadez, Agadez, Niger</addr-line></aff><aff id="aff2"><addr-line>LAPISEN, Ecole Doctorale Polytechnique, INPHB, Yamoussoukro, Cote d’ivoire</addr-line></aff><aff id="aff3"><addr-line>Département de Chimie, Faculté des Sciences et Technique, Université d’Agadez, Agadez, Niger</addr-line></aff><pub-date pub-type="epub"><day>02</day><month>06</month><year>2020</year></pub-date><volume>08</volume><issue>04</issue><fpage>197</fpage><lpage>204</lpage><history><date date-type="received"><day>15,</day>	<month>May</month>	<year>2020</year></date><date date-type="rev-recd"><day>14,</day>	<month>June</month>	<year>2020</year>	</date><date date-type="accepted"><day>17,</day>	<month>June</month>	<year>2020</year></date></history><permissions><copyright-statement>&#169; Copyright  2014 by authors and Scientific Research Publishing Inc. </copyright-statement><copyright-year>2014</copyright-year><license><license-p>This work is licensed under the Creative Commons Attribution International License (CC BY). http://creativecommons.org/licenses/by/4.0/</license-p></license></permissions><abstract><p>
 
 
  Ferrimagnetic materials such as natural magnetite are used for practical applications because of their electronic, magnetic and catalytic properties in the degradation of organic compounds. In order to determine its physicochemical properties in relation to its catalytic activity, the natural magnetite of Ofoud Mount (Niger) is characterized by X-ray florescence (XRF), X-ray diffraction (DRX), specific surface area (BET) and Fourier transformed infrared (FTIR). The result shows an iron content of 97.09% and a specific surface area of 69.742 m
  <sup>2</sup>/g. The crystal structure of magnetite is cubic with lattice parameters 
  α = 
  β = 
  γ = 90&amp;#176;, a (&amp;#197;) = b (&amp;#197;) = c (&amp;#197;) = 8.3740. The results of this study suggest that the natural magnetite of Ofoud Mount can be used as iron source in various fields of science despite the presence of a few impurities that can improve its catalytic activity.
 
</p></abstract><kwd-group><kwd>Magnetic</kwd><kwd> Mineral Composition</kwd><kwd> Structural</kwd><kwd> Surface Area</kwd></kwd-group></article-meta></front><body><sec id="s1"><title>1. Introduction</title><p>Ferrimagnetic materials such as natural magnetite are used widely in various fields of science because of their electronic, magnetic and catalytic properties [<xref ref-type="bibr" rid="scirp.100951-ref1">1</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref2">2</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref3">3</xref>]. Characterized by a magnetic susceptibility which allows their recovery after use, natural magnetite, magnetite fixed on a support and ferromagnetic nanoparticles are used as catalysts in environmental remediations because of their stability [<xref ref-type="bibr" rid="scirp.100951-ref4">4</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref5">5</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref6">6</xref>]. According to H. He et al. [<xref ref-type="bibr" rid="scirp.100951-ref7">7</xref>], natural magnetite exhibits catalytic performance superior to the pure synthetic magnetite. It also contains ferrous and ferric ions which improve its catalytic activity more than other ferromagnetic materials such as hematite and goethite which contain only ferric ion [<xref ref-type="bibr" rid="scirp.100951-ref8">8</xref>]. Due to its redox properties, magnetite offers high activity in the oxidation process of many non-biodegradable organic compounds (pentachorophenol, phenol, polycyclic aromatic compounds PAHs) [<xref ref-type="bibr" rid="scirp.100951-ref9">9</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref10">10</xref>]. Magnetics are ideal for treating soil contaminating with hydrocarbons through the heterogeneous Fenton reaction [<xref ref-type="bibr" rid="scirp.100951-ref11">11</xref>]. Many studies have demonstrated that the capacity of raw rocks rich in magnetite to adsorb and degrade pollutants is largely dependent on their mineral structure and composition [<xref ref-type="bibr" rid="scirp.100951-ref12">12</xref>]. It specifically depends on parameters such as the presence of impurities, the specific surface area, the oxidation state. The chemical composition of magnetite also varies from one iron ore to another, which gives it variable chemical properties [<xref ref-type="bibr" rid="scirp.100951-ref13">13</xref>]. The characterization of each raw rock is therefore essential for a better understanding of its properties and its use. Previous studies on general characterization have been carried out on raw rocks rich in magnetite [<xref ref-type="bibr" rid="scirp.100951-ref14">14</xref>], on purified materials [<xref ref-type="bibr" rid="scirp.100951-ref15">15</xref>] and synthesized magnetite [<xref ref-type="bibr" rid="scirp.100951-ref6">6</xref>]. The aim of this study was to characterize the iron mineral rich in magnetite collected from the Air massif at Ofoud Mount in relation to its catalytic activities.</p></sec><sec id="s2"><title>2. Material and Methods</title><p>The natural materials rich in magnetite used in this study was collected from the Air massif at Ofoud Mount [<xref ref-type="bibr" rid="scirp.100951-ref5">5</xref>]. These materials have been characterized after grinding and sieved through a mesh to obtain an average size of 0.05 mm [<xref ref-type="bibr" rid="scirp.100951-ref16">16</xref>]. The mineral composition of the raw magnetite was generated by X-ray fluorescence (XRF), the mineralogical analysis was done with the X-ray diffraction method (XRD) and the specific surface area by the standard BET method.</p></sec><sec id="s3"><title>3. Result and Discussion</title><sec id="s3_1"><title>3.1. Mineral Composition</title><p>The raw rock content (<xref ref-type="table" rid="table1">Table 1</xref>) indicated that iron is dominated by 97.09% (considered as Fe<sub>3</sub>O<sub>4</sub>) indicating a probable high content of magnetite and a low content of impurities. It is thus mainly composed of iron with trace elements (Ti, Ni, Co, Mn, Al and Mg). These elements had already been found in natural magnetite by Razjigaeva et al., 1992 [<xref ref-type="bibr" rid="scirp.100951-ref9">9</xref>]. Previous studies on synthetic magnetite have shown that the incorporation of Mn, Co, V, and Cr enhances the heterogeneous catalytic activity in the degradation of organic pollutants by hydrogen peroxide [<xref ref-type="bibr" rid="scirp.100951-ref3">3</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref10">10</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref17">17</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref18">18</xref>]. The chemical composition of the raw rock proves that it can be used as iron source in various fields of science. Some studies have shown that Ni has an inhibitory effect in the catalytic activity of the magnetite [<xref ref-type="bibr" rid="scirp.100951-ref19">19</xref>]. In the magnetite characterized in this study Ni content is very low.</p></sec><sec id="s3_2"><title>3.2. Structural Properties</title><p>The physical and chemical properties of natural magnetite depend also on its structure. The crystal structure and unit parameters of magnetite were studied at room temperature using an Empyreal X-ray diffractometer. The Mount Ofoud magnetite diffractogram is shown in <xref ref-type="fig" rid="fig1">Figure 1</xref>.</p><p>The XRD pattern is characterized by several reflections (<xref ref-type="fig" rid="fig1">Figure 1</xref>), the most intense occurred at the Position [˚2Th.] = 43.1763. <xref ref-type="fig" rid="fig1">Figure 1</xref> showed intense and sharp diffraction peaks attesting a high degree of crystallization [<xref ref-type="bibr" rid="scirp.100951-ref20">20</xref>]. The XRD measurements indicated that magnetite was the only crystalline phase detected despite the presence of the minor elements obtained by XRF analysis. Its structural formula is Fe<sub>24</sub>.<sub>00</sub> O<sub>32.00</sub> with scale fac of 0.773. The presence of a single phase can be explained by the fact that in natural magnetite, divalent cations (Co, Ni, Zn, Cu, Mn, etc.), trivalent cations (Al, V, Cr, etc.) and tetravalents (Ti) can substitute isomorphically for iron cations without modifying the reverse</p><table-wrap id="table1" ><label><xref ref-type="table" rid="table1">Table 1</xref></label><caption><title> Chemical composition of the raw rock</title></caption><table><tbody><thead><tr><th align="center" valign="middle"  rowspan="2"  >El&#233;ment</th><th align="center" valign="middle"  colspan="2"  >Raw Rock</th></tr></thead><tr><td align="center" valign="middle" >Ppm</td><td align="center" valign="middle" >Percent (%)</td></tr><tr><td align="center" valign="middle" >Co</td><td align="center" valign="middle" >1331.53</td><td align="center" valign="middle" >0.207631848</td></tr><tr><td align="center" valign="middle" >Ni</td><td align="center" valign="middle" >2007.27</td><td align="center" valign="middle" >0.313003221</td></tr><tr><td align="center" valign="middle" >Fe</td><td align="center" valign="middle" >622,636.38</td><td align="center" valign="middle" >97.09067165</td></tr><tr><td align="center" valign="middle" >Mn</td><td align="center" valign="middle" >168.84</td><td align="center" valign="middle" >0.02632803</td></tr><tr><td align="center" valign="middle" >Ti</td><td align="center" valign="middle" >4154.81</td><td align="center" valign="middle" >0.647879415</td></tr><tr><td align="center" valign="middle" >Mg</td><td align="center" valign="middle" >2177.01</td><td align="center" valign="middle" >0.339471592</td></tr><tr><td align="center" valign="middle" >TOTAL</td><td align="center" valign="middle" >632,475.84</td><td align="center" valign="middle" >100</td></tr></tbody></table></table-wrap><p>spinel structure [<xref ref-type="bibr" rid="scirp.100951-ref3">3</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref17">17</xref>]. According to Zhong et al. [<xref ref-type="bibr" rid="scirp.100951-ref21">21</xref>] with the increase of titanium content in the magnetite, the average particle size decreases and the size distribution becomes narrow. The low intensity peak at the position [˚2Th.] = 18.336 can thus be linked to the presence of titanium in the magnetite. The crystal structure of magnetite is cubic with lattice parameters α = β = γ = 90˚, a (&#197;) = b (&#197;) = c (&#197;) = 8.3740. The only magnetite phase detected crystalize in the Fd-3m with space number 227 [<xref ref-type="bibr" rid="scirp.100951-ref22">22</xref>]. The fit was satisfactory for the Fe<sub>3</sub>O<sub>4</sub> phase after introducing the atom coordinates (<xref ref-type="table" rid="table1">Table 1</xref>). Its density of 5.24 g/cm<sup>3</sup> was appropriate with previous research [<xref ref-type="bibr" rid="scirp.100951-ref23">23</xref>]. The result of the DRX analysis shows the chemical purity of this natural magnetite.</p></sec><sec id="s3_3"><title>3.3. Specific Surface</title><p>In the heterogeneous Fenton process, the reaction between ferrous or ferric ions and hydrogen peroxide the active sites are located on the surface of the catalyst [<xref ref-type="bibr" rid="scirp.100951-ref24">24</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref25">25</xref>]. The specific surface of the magnetite was determined by N2-BET multipoint analysis using a Novantin kantachrome type surface analyzer.</p><p>As can be seen in <xref ref-type="table" rid="table3">Table 3</xref>, eight methods were used to determine the surface area of the magnetite. Among these analyses, BET is the most popular which has been successfully proved in evaluating the specific area of materials. The main surface area was determined to be 69.742 m<sup>2</sup>/g with Multi Points BET (<xref ref-type="fig" rid="fig2">Figure 2</xref>). The relatively high value obtained by adsorption of nitrogen on the magnetite powder is similar to other researches Gorski et al. [<xref ref-type="bibr" rid="scirp.100951-ref22">22</xref>] for a synthetic magnetite. Compared to the specific surface of pure magnetite obtained by several authors, this surface is relatively high [<xref ref-type="bibr" rid="scirp.100951-ref26">26</xref>] [<xref ref-type="bibr" rid="scirp.100951-ref27">27</xref>]. The high value may be related to the presence of titanium in the magnetite because it is approximately equal to the titanomagnetite surface area obtained by Zhong et al. [<xref ref-type="bibr" rid="scirp.100951-ref21">21</xref>]. During the heteroge-</p><table-wrap id="table2" ><label><xref ref-type="table" rid="table2">Table 2</xref></label><caption><title> Atom coordinates of Fe<sub>3</sub>O<sub>4</sub></title></caption><table><tbody><thead><tr><th align="center" valign="middle" >NO.</th><th align="center" valign="middle" >Name</th><th align="center" valign="middle" >Element</th><th align="center" valign="middle" >X</th><th align="center" valign="middle" >Y</th><th align="center" valign="middle" >Z</th><th align="center" valign="middle" >Biso</th><th align="center" valign="middle" >Sof</th><th align="center" valign="middle" >Wyck</th></tr></thead><tr><td align="center" valign="middle" >1 2 3</td><td align="center" valign="middle" >FE1 FE2 O</td><td align="center" valign="middle" >Fe Fe O</td><td align="center" valign="middle" >0.37500 0.00000 0.24600</td><td align="center" valign="middle" >0.37500 0.00000 0.24600</td><td align="center" valign="middle" >0.37500 0.00000 0.24600</td><td align="center" valign="middle" >0.8504 1.0399 0.7604</td><td align="center" valign="middle" >1.0000 1.0000 1.0000</td><td align="center" valign="middle" >8b 16c 32e</td></tr></tbody></table></table-wrap><table-wrap id="table3" ><label><xref ref-type="table" rid="table3">Table 3</xref></label><caption><title> Comparison on results of surface area by different methods</title></caption><table><tbody><thead><tr><th align="center" valign="middle" >Method</th><th align="center" valign="middle" >S (m<sup>2</sup>/g)</th></tr></thead><tr><td align="center" valign="middle" >Single point BET</td><td align="center" valign="middle" >4.320e+01</td></tr><tr><td align="center" valign="middle" >Multi Points BET</td><td align="center" valign="middle" >6.974e+01</td></tr><tr><td align="center" valign="middle" >Langmuir surface area</td><td align="center" valign="middle" >3.644e+02</td></tr><tr><td align="center" valign="middle" >BJH method cumulative adsorption surface area</td><td align="center" valign="middle" >7.990e+01</td></tr><tr><td align="center" valign="middle" >DH method cumulative adsorption surface area</td><td align="center" valign="middle" >8.512e+01</td></tr><tr><td align="center" valign="middle" >T method external surface area</td><td align="center" valign="middle" >6.974e+01</td></tr></tbody></table></table-wrap><p>neous Fenton process, the reaction between ferrous and ferric ions with hydrogen peroxide occurs on the surface of the catalyst [<xref ref-type="bibr" rid="scirp.100951-ref25">25</xref>]. The high specific surface of the crushed magnetite can thus favor the oxidation of the adsorbed compounds. The cumulative pore size distribution for magnetite is shown in <xref ref-type="fig" rid="fig3">Figure 3</xref>. It shows that the micropores vary from 1.6 to 6.0 nm. The average pore diameter estimated from the peak position is around 2.8 nm [<xref ref-type="bibr" rid="scirp.100951-ref8">8</xref>]. The most of the pore volume is in the mesoporous range (2 to 10 nm), showing the strong porous structure of the magnetite. The BET surface area and the average pores diameter values show that it can be used for pollutants adsorption.</p></sec></sec><sec id="s4"><title>4. Conclusion</title><p>This study demonstrates that the natural magnetite from Ofoud mount is highly pure materials which can be used in various fields of science. The XRD analysis showed that magnetite is the only phase detected despite the presence of traces elements (generated by XRF) that can improve its catalytic activities.</p></sec><sec id="s5"><title>Acknowledgements</title><p>The authors would like to express their sincere and honest gratitude to the Agadez University.</p></sec><sec id="s6"><title>Conflicts of Interest</title><p>The authors declare no conflicts of interest regarding the publication of this paper.</p></sec><sec id="s7"><title>Cite this paper</title><p>Aziz, M.S.A., Kopoin, A. and Sani, O.M. (2020) Compositional, Structural, Surface Characterizations of Natural Magnetite from Air Massif (Niger) in Relation to Its Catalytic Activity. 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