skip to main content

Synthesis and Characterization of Hematite (α-Fe₂O₃) Nanomaterials from Red Mud Using EDTA as Capping Agent

1Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Tanjungpura, Pontianak, West Kalimantan, Indonesia

2Department of Electrical Engineering, Faculty of Engineering, Universitas Tanjungpura, Pontianak, West Kalimantan, Indonesia

Received: 9 Jul 2025; Revised: 28 Oct 2025; Accepted: 29 Oct 2025; Published: 31 Oct 2025.
Open Access Copyright 2025 Jurnal Kimia Sains dan Aplikasi under http://creativecommons.org/licenses/by-sa/4.0.

Citation Format:
Cover Image
Abstract
Hematite (α-Fe2O3) nanomaterials, a stable phase of iron oxide, hold significant potential for diverse materials science and technology applications. In this study, red mud was employed as a low-cost precursor for synthesizing hematite nanomaterials, with ethylenediaminetetraacetic acid (EDTA) used as a capping agent to prevent particle agglomeration. The effect of EDTA on particle size and colloidal stability was investigated by comparing three synthesis variations: (a) without EDTA (NPH-1), (b) with EDTA via the precipitation method (NPH-2), and (c) with EDTA via the hydrothermal method (NPH-3). XRD analysis confirmed the formation of crystalline hematite (α-Fe2O3) in all samples. FT-IR spectroscopy revealed absorption bands at 1624 cm−1 and 1382 cm−1, corresponding to the symmetric and asymmetric stretching vibrations of the carboxylate (COO) group, respectively. The difference in these wavenumbers suggests monodentate coordination between the carboxyl groups of EDTA and the hematite nanoparticle surfaces. Particle size analysis indicated that the EDTA-assisted synthesis via precipitation (NPH-2) produced the smallest average particle size (149.6 nm) with a narrow size distribution, as reflected by a polydispersity index (PDI) of 0.43. Furthermore, this sample demonstrated enhanced colloidal stability with a zeta potential of −34.0 mV. These findings suggest that the synthesized α-Fe2O3 nanomaterials produced with narrow particle size distribution and high colloidal stability, are promising for visible-light photocatalysis.
Fulltext View|Download
Keywords: Capping agent; EDTA; Hematite nanomaterial; Iron Oxide; Red Mud

Article Metrics:

  1. Vancha Harish, Md Mustafiz Ansari, Devesh Tewari, Manish Gaur, Awadh Bihari Yadav, María-Luisa García-Betancourt, Fatehy M. Abdel-Haleem, Mikhael Bechelany, Ahmed Barhoum, Nanoparticle and Nanostructure Synthesis and Controlled Growth Methods, Nanomaterials, 12, 18, (2022), 3226 https://doi.org/10.3390/nano12183226
  2. Amanullakhan Pathan, Sandip H. Bhatt, Shailesh Vajapara, C. P. Bhasin, Solar light induced photo catalytic properties of α-Fe2O3 nanoparticles for degradation of methylene blue dye, International Journal of Thin Film Science and Technology, 11, 2, (2022), 213-224
  3. Ahmad Fajri Soekansa, Nafis Sudirman, Syamsi Aini, Sintesis dan Karakterisasi Pigmen Merah Hematit (α-Fe2O3) dari Pasir Besi Kabupaten Sijunjung, Sumatera Barat, Indonesia, Periodic, 12, 1, (2023), 9-13 https://doi.org/10.24036/p.v12i1.115856
  4. Mastuki Mastuki, A. W. Brata, A. G. Istiawan, B. Aditya, H. Masrufi, Study Experimental The Effect of CaCO3 and Fe2O3 Mass Composition Ratio on Calcium Ferrite Phase Formation Base on Local Materials Iron Sand and Limestone, SINTEK JURNAL: Jurnal Ilmiah Teknik Mesin, 14, 1, (2020), 27-31 https://doi.org/10.24853/sintek.14.1.27-31
  5. Jingyi Wang, Panpan Sun, Huimin Xue, Jinxiu Chen, Heng Zhang, Wancheng Zhu, Red mud derived facile hydrothermal synthesis of hierarchical porous α-Fe2O3 microspheres as efficient adsorbents for removal of Congo red, Journal of Physics and Chemistry of Solids, 140, (2020), 109379 https://doi.org/10.1016/j.jpcs.2020.109379
  6. Zahra Karimi, Ahmad Rahbar-Kelishami, Efficient utilization of red mud waste via stepwise leaching to obtain α-hematite and mesoporous γ-alumina, Scientific Reports, 13, 1, (2023), 8527 https://doi.org/10.1038/s41598-023-35753-w
  7. Indi Rizki Wahyinto, Anthoni B. Aritonang, Titin Anita Zaharah, Extraction and Characterization of Fe2O3 from Red Mud PT. Indonesia Chemical Alumina West Kalimantan, Berkala Sainstek, 10, 3, (2022), 155-161 https://doi.org/10.19184/bst.v10i3.30252
  8. Pratibha Sharma, Sujata Kumari, Debasree Ghosh, Vandana Yadav, Ankush Vij, Pooja Rawat, Shalendra Kumar, Chittaranjan Sinha, Sonia Saini, Vivek Sharma, Md Imtaiyaz Hassan, Chandra Mohan Srivastava, Sudip Majumder, Capping agent-induced variation of physicochemical and biological properties of α-Fe2O3 nanoparticles, Materials Chemistry and Physics, 258, (2021), 123899 https://doi.org/10.1016/j.matchemphys.2020.123899
  9. Namra Abid, Aqib Muhammad Khan, Sara Shujait, Kainat Chaudhary, Muhammad Ikram, Muhammad Imran, Junaid Haider, Maaz Khan, Qasim Khan, Muhammad Maqbool, Synthesis of nanomaterials using various top-down and bottom-up approaches, influencing factors, advantages, and disadvantages: A review, Advances in Colloid and Interface Science, 300, (2022), 102597 https://doi.org/10.1016/j.cis.2021.102597
  10. Rabia Javed, Muhammad Zia, Sania Naz, Samson O. Aisida, Noor ul Ain, Qiang Ao, Role of capping agents in the application of nanoparticles in biomedicine and environmental remediation: recent trends and future prospects, Journal of Nanobiotechnology, 18, 1, (2020), 172 https://doi.org/10.1186/s12951-020-00704-4
  11. Vidya Devadiga, Geetha M. Pinto, Ronald Nazareth, K. Amrutha, Synthesis of functionalized α -Fe2O3 nanoparticles: Characterization and applications, Materials Today: Proceedings, (2023), https://doi.org/10.1016/j.matpr.2023.05.111
  12. Berlian Sitorus, Mincen Reva, Intan Syahbanu, Extraction of Scandium and Removal of Iron from Bauxite Residue using Hydrochloric Acid Solution with/without Addition of EDTA, Reaktor, 24, 3, (2025), 76-81 https://doi.org/10.14710/reaktor.24.3.76-81
  13. Pratishtha Kushwaha, Pratima Chauhan, Synthesis of spherical and Rod-Like EDTA assisted α-Fe2O3 nanoparticles via Co-precipitation method, Materials Today: Proceedings, 44, (2021), 3086-3090 https://doi.org/10.1016/j.matpr.2021.02.450
  14. Titin Anita Zaharah, Wanda Rossalina, Imelda Hotmarisi Silalahi, Komposisi Unsur dan Karakterisasi Mineral Magnetik dalam Red Mud, Residu Bauksit di PT. Indonesia Chemical Alumina (ICA) Kalimantan Barat (Elemental Composition And Mineral Characteristics of Magnetic Red Mud, Bauxite Residue at PT. Indonesia Chemical Alumina (ICA), West Kalimantan), Indonesian Journal of Pure and Applied Chemistry, 4, 3, (2021), 139-144 https://doi.org/10.26418/indonesian.v4i3.49660
  15. G. Svehla, Vogel's Textbook of Macro and Semimicro Qualitative Inorganic Analysis, Longman, 1985,
  16. Yong Richard Sriwijaya, Paramita Jaya Ratri, Tirta Rona Mayangsari, Azis Adharis, Shabrina Sri Riswati, Synthesis of Iron Oxide (Fe2O3)-Xanthan Gum Nanoparticle Composites Its Potential as a Chemical Flooding Media in Enhanced Oil Recovery (EOR), Jurnal Kimia Valensi, 9, 1, (2023), 53-58 https://doi.org/10.15408/jkv.v9i1.29468
  17. V. Archana, J. Joseph Prince, S. Kalainathan, Simple One-Step Leaf Extract-Assisted Preparation of α-Fe2O3 Nanoparticles, Physicochemical Properties, and Its Sunlight-Driven Photocatalytic Activity on Methylene Blue Dye Degradation, Journal of Nanomaterials, 2021, 1, (2021), 8570351 https://doi.org/10.1155/2021/8570351
  18. Pantharee Kongsat, Kobkun Kudkaew, Jiratikul Tangjai, Edgar A. O'Rear, Thirawudh Pongprayoon, Synthesis of structure-controlled hematite nanoparticles by a surfactant-assisted hydrothermal method and property analysis, Journal of Physics and Chemistry of Solids, 148, (2021), 109685 https://doi.org/10.1016/j.jpcs.2020.109685
  19. Hikaru Sawai, Ismail M. M. Rahman, Mayuko Fujita, Naoyuki Jii, Tomoya Wakabayashi, Zinnat A. Begum, Teruya Maki, Satoshi Mizutani, Hiroshi Hasegawa, Decontamination of metal-contaminated waste foundry sands using an EDTA–NaOH–NH3 washing solution, Chemical Engineering Journal, 296, (2016), 199-208 https://doi.org/10.1016/j.cej.2016.03.078
  20. Amanda Kulpa, Jacek Ryl, Grzegorz Skowierzak, Adrian Koterwa, Grzegorz Schroeder, Tadeusz Ossowski, Paweł Niedziałkowski, Comparison of Cadmium Cd2+ and Lead Pb2+ Binding by Fe2O3@SiO2-EDTA Nanoparticles – Binding Stability and Kinetic Studies, Electroanalysis, 32, 3, (2020), 588-597 https://doi.org/10.1002/elan.201900616
  21. A. G. Magdalena, I. M. B. Silva, R. F. C. Marques, A. R. F. Pipi, P. N. Lisboa-Filho, M. Jafelicci, EDTA-functionalized Fe3O4 nanoparticles, Journal of Physics and Chemistry of Solids, 113, (2018), 5-10 https://doi.org/10.1016/j.jpcs.2017.10.002
  22. Eduwin Saputra, A colorimetric detection of creatinine based-on EDTA capped-gold nanoparticles (EDTA-AuNPs): Digital Image Colorimetry, Sensors International, 5, (2024), 100286 https://doi.org/10.1016/j.sintl.2024.100286
  23. Maryam Jouyandeh, Mohammad Reza Ganjali, Jagar A. Ali, Mustafa Aghazadeh, Isa Karimzadeh, Krzysztof Formela, Xavier Colom, Javier Cañavate, Mohammad Reza Saeb, Curing epoxy with ethylenediaminetetraacetic acid (EDTA) surface-functionalized CoxFe3-xO4 magnetic nanoparticles, Progress in Organic Coatings, 136, (2019), 105248 https://doi.org/10.1016/j.porgcoat.2019.105248
  24. Ekta Shah, Pratik Upadhyay, Mala Singh, Mohmmad Shoab Mansuri, Rasheedunnisa Begum, Navin Sheth, Hemant P. Soni, EDTA capped iron oxide nanoparticles magnetic micelles: drug delivery vehicle for treatment of chronic myeloid leukemia and T1–T2 dual contrast agent for magnetic resonance imaging, New Journal of Chemistry, 40, 11, (2016), 9507-9519 https://doi.org/10.1039/c6nj00655h
  25. Abdenacer Benhammada, Djalal Trache, Mohamed Kesraoui, Ahmed Fouzi Tarchoun, Salim Chelouche, Abderrahmane Mezroua, Synthesis and characterization of α-Fe2O3 nanoparticles from different precursors and their catalytic effect on the thermal decomposition of nitrocellulose, Thermochimica Acta, 686, (2020), 178570 https://doi.org/10.1016/j.tca.2020.178570
  26. Diaa Eldin Fouad, Chunhong Zhang, Hamdy El-Didamony, Liu Yingnan, Tadele Daniel Mekuria, Ahmer Hussain Shah, Improved size, morphology and crystallinity of hematite (α-Fe2O3) nanoparticles synthesized via the precipitation route using ferric sulfate precursor, Results in Physics, 12, (2019), 1253-1261 https://doi.org/10.1016/j.rinp.2019.01.005
  27. Camilah D. Powell, Amanda W. Lounsbury, Zachary S. Fishman, Christian L. Coonrod, Miranda J. Gallagher, Dino Villagran, Julie B. Zimmerman, Lisa D. Pfefferle, Michael S. Wong, Nano-structural effects on Hematite (α-Fe2O3) nanoparticle radiofrequency heating, Nano Convergence, 8, 1, (2021), 8 https://doi.org/10.1186/s40580-021-00258-7
  28. Adwitiya Chakraborty, Prasanta Kumar Sinha, Milan Kanti Naskar, Low Temperature Processing of Iron Oxide Nanoflakes from Red Mud Extract toward Favorable De-arsenification of Water, ACS Omega, 8, 32, (2023), 29281-29291 https://doi.org/10.1021/acsomega.3c02689
  29. Thandi B. Mbuyazi, Peter A. Ajibade, Influence of Different Capping Agents on the Structural, Optical, and Photocatalytic Degradation Efficiency of Magnetite (Fe3O4) Nanoparticles, Nanomaterials, 13, 14, (2023), 2067 https://doi.org/10.3390/nano13142067

Last update:

No citation recorded.

Last update: 2025-11-12 07:54:44

No citation recorded.