Scholarly article on topic 'Synthesis and Characterizatation of Magnetite Nanoparticle Coated Humic Acid (Fe3O4/HA)'

Synthesis and Characterizatation of Magnetite Nanoparticle Coated Humic Acid (Fe3O4/HA) Academic research paper on "Materials engineering"

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{synthesis / characterization / magnetite / "humic acids" / "peat soil"}

Abstract of research paper on Materials engineering, author of scientific article — Soerja Koesnarpadi, Sri Juari Santosa, Dwi Siswanta, Bambang Rusdiarso

Abstract Magnetite nanoparticles (Fe3O4) coated humic acids (HA) by a co-precipitation method using ammonium hydroxide. The HA was extracted from peat soil of Sambutan, East Kalimantan, Indonesia and then have been succesfully coated onto the surface of Fe3O4. Characterization of FT-IR spectra indicate that the coating Fe3O4/HA have been bound by Fe-COOR chemical bond. The XRD measurements does not affect the crystals structure. Scanning electron microscopy revealed the magnetic particle size is almost homogenous of 10-18nm. Both of Fe3O4 and the coating Fe3O4/HA were of the cubic spinel structure and spherical-shaped morphology. The modification of HA on Fe3O4 can decrease the saturation magnetization from 71.3 emu/g to 69.5 emu/g.

Academic research paper on topic "Synthesis and Characterizatation of Magnetite Nanoparticle Coated Humic Acid (Fe3O4/HA)"

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Procedía Environmental Sciences 30 (2015) 103-108

International Conference on Environmental Forensics 2015 (iENFORCE2015)

Synthesis and characterizatation of magnetite nanoparticle coated

humic acid (Fe3O4/HA)

Soerja Koesnarpadi , Sri Juari Santosa , Dwi Siswanta , Bambang Rusdiarso

a Department of Chemistry, Mathematics and Natural Sciences, Mulawarman University, Samarinda, 75119, Indonesia b Department of Chemistry, Mathematics and Natural Science,s Gadjah Mada University, Yogyakarta 54123, Indonesia

Abstract

Magnetite nanoparticles (Fe3O4) coated humic acids (HA) by a co-precipitation method using ammonium hydroxide. The HA was extracted from peat soil of Sambutan, East Kalimantan, Indonesia and then have been succesfully coated onto the surface of Fe3O4. Characterization of FT-IR spectra indicate that the coating Fe3O4/HA have been bound by Fe-COOR chemical bond. The XRD measurements does not affect the crystals structure. Scanning electron microscopy revealed the magnetic particle size is almost homogenous of 10-18 nm. Both of Fe3O4 and the coating Fe3O4/HA were of the cubic spinel structure and spherical-shaped morphology. The modification of HA on Fe3O4 can decrease the saturation magnetization from 71.3 emu/g to 69.5 emu/g.

© 2015The Authors.PublishedbyElsevierB.V This is an open access article under the CC BY-NC-ND license (http://creativecommons.Org/licenses/by-nc-nd/4.0/).

Peer-reviewunderresponsibilityoforganizingcommittee of Environmental Forensics Research Centre, Faculty of Environmental Studies, Universiti Putra Malaysia.

Keywords: synthesis; characterization; magnetite; humic acids; peat soil

1. Introduction

Magnetite nanoparticles (Fe3O4) have unique size, physical properties and potencial applications in biomedical, biotechnology, materials sciences, engineering and environmental. The most studied materials due to their response to magnetic field, high saturation magnetization, non-toxic and biocompatible[1,2]. The magnetite nanoparticles are susceptible to air oxidation and easily aggregated in aqueous system Thus, the stabilization of magnetite is desirable [3,4.]

* Corresponding author. Tel.: +62-81347466457; fax: +62-0541-747974 E-mail address:soerja.koes@gmail .com

1878-0296 © 2015 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Peer-review under responsibility of organizing committee of Environmental Forensics Research Centre, Faculty of Environmental Studies,

Universiti Putra Malaysia.

doi:10.1016/j.proenv.2015.10.018

The humic acids (HA) are natural macromolecular compound with multi functional group dominated by carboxyl and hydroxyl group. The functional group on HA possess different ability in binding metal ion through complex formation [5]. The Indonesian terrestrial HA were very specific in their oxygen containing principal aims of this study are to characterize the groundwater hydrochemistry in different monsoon seasons and to determine the extents of saltwater intrusion in Kapas Island aquifer based on the ionic strength of selected ions.

Coating of particle surface can effectively prevent the adhesion of colliding particles during thermal motion. Binding HA on Fe3O4 influences the sorption because the adsorption of HA result polyanionic organic coating on Fe3O4 and thus essentially altering the surface properties. The adsorption capacity for metal cations with complex HA and Fe3O4 was reported to be larger than that with the respective HA or Fe3O4 alone [6,7,8]. Recent research indicated HA has high affinity to Fe3O4 nanoparticles enhanced the stability of nano dispersion by preventing their aggregation [9,10].

In this work, we developed the coating Fe3O4/HA using humic acid from peat soil of Sambutan, East Kalimatan on Fe3O4 by co-precipitation methods and characterization of spectrum consist of functional groups, crystal structure, morphologys, dispersion and size distribution and magnetic properties were investigated.

2. Methods

2.1. Study site

The reagents of analytical grade i.e., FeCl3.6.H2O, FeSO4.7.H2O, NH4OH 25%, C6H5OH, HCl, HF, H2O2, NaOH, N2.

2.2. Extraction and purification of HA from Sambutan village, Samarinda, East Kalimantan

The humic acid (HA) was extracted of peat soil in 0.1 M NaOH under nitrogen atmosphere at ambient temperature with and mechanical stirring overnight. The suspension was centrifugated and then filterred and the filtrate was precipitated with 6 HCl. The precipitated was centrifugated then precipitate was purified with HCl and HF. The HA obtained were washed with distilled water and dried in vacuum.

2.3. Preparations and characterization of Fe3O/HA

The coating Fe3O4/HA was prepared by the co-precipitation method, FeCl3.6.H2O and FeSO4.7H2O were dissolved into 25 mL water and heated to 90 oC. Then added of NH4OH 25% until pH 11 and 0.125 g of humic acids sodium salt dissolved in 12.5 mL of water were added rapidly and sequestially. The mixture was aged at 90 oC for 30 minutes and then cooled to room temperature. The black precipitate was separated from solution and washed to neutral with water. The functional group of Fe3O4/HA, Fe3O4 and HA were characterized by Fourier transform spectrometer (FT-IR) 8201 PC Shimadzu. The crystal structure was analyzed by X-ray difraction (XRD) Shimadzu using CuKa radiation (X=1.5406 A) operated at 40kV and 30 mA.. The size and morphologies of nanoparticles were determined by Transmition electron microscopy (TEM, JEOL JEM 1400). The magnetic nanoparticles properties were measured by Vibrating sample magnetometer (VSM, Oxford).

3. Results and discussion

The magnetite is an amphoteric solids, which can develop charges in the protonation and deprotonation reaction of Fe-OH sites on surface. This process is controlled by the pH and ion strength in aqueous medium. At pH lower than the PZC (pH < 7.9) the surface charge is positive, electrostatic interaction between HA and Fe3O4 is and dominant under acidic conditions.

Fe-OH2+ + R-COO- Fe-OOC-R + H2O (1)

At above the pH of PZC (pH > 7.9) the surface charge is negative, the coating HA on Fe3O4 in alkaline condition, the dominant interaction between HA and Fe3O4 is probable a ligand-change reaction with surface hydroxyl [7,9].

Fe-OH + R-COO- Fe-OOC-R + OH- (2)

Identification of functional group of HA from peat soil of Sambutan village, East Kalimantan, Indonesia was presence of O-H stretching (3425 cm-1). The absorption band at 2924 cm-1 was stretching vibration of aliphatic C-H in CH2 or/and CH3, wavenumber 1706 cm-1 and 1627 cm-1 were attributed to the streching C=O of COOH and COO-asymmetric stretching vibrations and streching of aromatic C=C, respectively. The FTIR spectra of Fe3O4 and Fe3O4/HA centered at 563 cm-1 were attributed to the stretching vibration of Fe-O bond. Succesfully coating of Fe3O4/HA shows the C=O stretching at 1404 cm-1, indicating the carboxylate anion interacting with FeO as the C=O stretches in free carboxylate acids (Fig.1) [8,9,10].

Wavelength number (1/cm)

Fig 1. FTIR Spectra of humic acid (HA) from Sambutan village, Samarinda, East Kalimantan (a), Fe3O4 (b) and Fe3O4/HA (c)

The XRD measurement was used to identify the crystalline structure of the product. The XRD patterns of Fe3O4/HA and Fe3O4 are shown in Fig 2.

0 10 20 30 40 50 60 70

2 theta

Fig 2. XRD pattern of humic acid (HA) from Sambutan village, Samarinda, East Kalimantan (a), Fe3O4 (b) and Fe3O4/HA (c)

Two materials had similar diffraction peaks at 29 = 30,1°, 35,4°, 43,1°, 57,0°, 62,68° dan 74,5°. The XRD peaks can match well with the characteristic peaks of inverse cubic spinel structure (JCPDS 19-0629). This result indicated that the crystal structure of Fe3O4.was not changed after modification with HA [2,11]. The average crystallite d calculated using the Debye-Scherrer equation d = KX/(Pcos9) are abaout Fe3O4 = 13.46 nm and Fe3O4/HA = 10.80

The morphology and mean particles size of these samples characterized by SEM (Fig. 3). The SEM images of HA was colloid-rigid shape. The magnetite shown homogenously spherical-shape and had distribution of particles size between 10-18 nm. This result is in agreement with the result of XRD analysis. The HA modified Fe3O4 shown coverage of HA on the surface Fe3O4 that significantly increased in the size and also well dispersed, which indicated HA efficiently reduces their aggregation [12]. Composition of C and O at magnetite coated HA was increased and then Fe was decreased after coating Fe3O4/HA.

Fig. 3. SEM images of humic acids (a), Fe3O4 (b) and humic acid coated Fe3O4 (Fe3O4/HA)

Table 1

No composition of element (%mass) HA Fe3O4 FeM/HA

1 C 63,44 2,69 5,91

2 O 33,79 8,40 10,53

3 Fe 2,77 88,91 83,57

The comparasion of saturation magnetization (M) of Fe3O4 and after magnetite coated HA at Fig 4. The saturation magnetization of Fe3O4 higher than magnetite coated HA, 71.3 emu/g and 69.5 emu/g. This saturation magnetization decreases evidently when Fe3O4 were modified with HA because attribute to the surface small particle spin effect which result in the reduction of magnetic moments of magnetite.

Fig 4. Magnetization curve of Fe3O4 (a) and Fe3O4/HA (b)

4. Conclusion

The magnetite coated HA could be success to synthezed with the FT-IR spectra reveals that HA have been successfully coated onto surface of Fe3O4 by chemical bond. The modification HA on Fe3O4 does not affect the crystals structure, decrease the saturation magnetization and excellent dispersion, which. indicated HA efficiently reduces their aggregation.

Acknowledgements

We gratefully acknowledge the Ministry of Higher Education, Republic of Indonesia for providing financial support the study of postgraduate in Universitas Gadjah Mada.

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