JURNAL ILMIAH Jumlah Penulis Status Pengusul Identitas

LEMBAR

HASIL PENILAIAN SEJAWAT SEBIDANG ATAU PEER REVIEW

KARYA ILMIAH : JURNAL ILMIAH

Judul Jurnal Ilmiah (Artikel) : Microstructure Characterization of Natural Magnetite from Sand Marina Beach By High Energy

Milling

Jumlah Penulis : 4 orang

Status Pengusul : Penulis Utama

Identitas Jurnal Ilmiah : a. Nama Jurnal : ORIENTAL JOURNAL OF CHEMISTRY An International

Open Free Access, Peer Reviewed Research Journal

b. Nomor ISSN : 0970-020 X

c. Vol, No., Bln Thn : Vol. 34, No.(2): Page. 868-874, 2018

d. Penerbit : Oriental Scientific Publishing Company

e. DOI artikel (jika ada) : http://dx.doi.org/10.13005/ojc/340234

f. Alamat web jurnal : http://www.orientjchem.org/vol34no2/microstructure-

characterization-of-natural-magnetite-from-sand-

marina-beach-by-high-energy-milling/

Alamat Artikel : http://www.orientjchem.org/download/45136 atau

https://doc-

pak.undip.ac.id/2894/1/OJC_Vol34_No2_p_868-

874.pdf Url Turnitin: (8%)

https://doc-pak.undip.ac.id/3033/2/Turnitin2.pdf

g. Terindex : Jurnal Internasional Bereputasi (Q4) terindeks SCOPUS

(SJR=0,17)

Kategori Publikasi Jurnal Ilmiah : Jurnal Ilmiah Internasional

(beri pada kategori yang tepat) Jurnal Ilmiah Nasional Terakreditasi

Jurnal Ilmiah Nasional Tidak Terakreditasi

Hasil Penilaian Peer Review :

Komponen

Yang Dinilai

Nilai Maksimal Jurnal Ilmiah

Nilai Akhir

Yang

Diperoleh

Internasional

Nasional

Terakreditasi

Nasional

Tidak

Terakreditasi

a. Kelengkapan unsur isi jurnal (10%) 4,00 4

b. Ruang lingkup dan kedalaman

pembahasan (30%)

12,00 12

c. Kecukupan dan kemutahiran

data/informasi dan metodologi (30%)

12,00 12

d. Kelengkapan unsur dan kualitas

terbitan/jurnal (30%)

12,00 10

Total = (100%) 40,00 38

Penulis Utama: 0,6 x 38 = 22,8

Catatan Penilaian artikel oleh Reviewer :

1. Kesesuaian dan kelengkapan unsur isi jurnal:

Isi jurnal sudah memenuhi kelengkapan subuah jurnal ilmiah (terindeks Scopus dan mempunya indeks SJR 0,17,

unsur-unsur jurnal juga sudah sesuai dan sinkron. Judul abstak, pendahuluan sampai kesimpulan lengkap. Nilai 4

2. Ruang lingkup dan kedalaman pembahasan:

Ruang lingkup pembahasan pada makalah ini sudah baik. Metode penelitian dan hasil disampaikan dengan mendalam

dan didukung oleh referensi yang memadai. Nilai 12

3. Kecukupan dan kemutakhiran data/informasi dan metodologi:

Metode yang digunakan merupakan metode yang terkikni dan disampaikan dengan jelas, referensi yang digunakan

sudah mencukupi dan mutakhir. Nilai 12

4. Kelengkapan unsur dan kualitas terbitan:

Kelengkapan dan kualitas terbitan sudah mencukupi dan suah terindeks di Scopus dan juga memiliki indeks SJR

0,17. Nilai 10

Semarang, 30 Maret 2020

Reviewer 1

Dr. Bambang Cahyono

NIP. 196303161988101001

Unit Kerja : Departemen Kimia FSM UNDIP

V

http://dx.doi.org/10.13005/ojc/340234

http://www.orientjchem.org/vol34no2/microstructure-characterization-of-natural-magnetite-from-sand-marina-beach-by-high-energy-milling/



http://www.orientjchem.org/download/45136

https://doc-pak.undip.ac.id/2894/1/OJC_Vol34_No2_p_868-874.pdf




LEMBAR




Milling













https://doc-





(SJR=0,17)





Komponen

Yang Dinilai

Nilai Maksimal Jurnal Ilmiah

Nilai Akhir

Yang

Diperoleh

Internasional

Nasional

Terakreditasi

Nasional

Tidak

Terakreditasi

e. Kelengkapan unsur isi jurnal (10%) 4,00 4

f. Ruang lingkup dan kedalaman

pembahasan (30%)

12,00 10

g. Kecukupan dan kemutahiran

data/informasi dan metodologi (30%)

12,00 12

h. Kelengkapan unsur dan kualitas

terbitan/jurnal (30%)

12,00 11

Total = (100%) 40,00 37

Penulis Utama: 0,6 x 37 = 22,2

Catatan Penilaian artikel oleh Reviewer :

1. Kesesuaian dan kelengkapan unsur isi jurnal:

Jurnal memiliki unsur yang lengkap sebagai standar jurnal internasional. Nilai 4

2. Ruang lingkup dan kedalaman pembahasan:

Ruang lingkup mengenai kimia material yang dibuat mikro dengan Ball milling, tetapi secara kimia kurang terlihat

hasilnya, pembahasan tidak disertai sitasi referensi sebelumnya. Nilai 10

3. Kecukupan dan kemutakhiran data/informasi dan metodologi:

Kuantitas dan kualitas pustaka baik, metodologi dapat dipahami pembaca. Nilai 12

4. Kelengkapan unsur dan kualitas terbitan:

Beberapa tulisan ada yang salah tulis (typo), kualitas terbitan cukup baik. Nilai 11


Reviewer 2

Drs. Gunawan, M.Si, Ph.D

NIP.196408251991031001


V










LEMBAR




Milling













https://doc-





(SJR=0,17)





Komponen

Yang Dinilai

Nilai Reviewer

Nilai Rata-rata Reviewer I Reviewer II

a. Kelengkapan unsur isi jurnal (10%) 4 4 4

b. Ruang lingkup dan kedalaman pembahasan (30%) 12 10 11

c. Kecukupan dan kemutahiran data/informasi dan

metodologi (30%)

12 12 12

d. Kelengkapan unsur dan kualitas terbitan/jurnal (30%) 10 11 10,5

Total = (100%) 38 37 37,5

Penulis Utama (rata-rata): 0,6 x 37,5 = 22,5


Reviewer 2

Drs. Gunawan, M.Si, Ph.D

NIP.196408251991031001


Reviewer 1

Dr. Bambang Cahyono

NIP. 196303161988101001











10/15/2020 TOC : Oriental Journal of Chemistry

www.orientjchem.org/toc/?vol=34&no=2 1/10

ISSN : 0970 - 020X, ONLINE ISSN : 2231-5039

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TOC Volume 34 Number 2

A Decade of Development of Ethylidenethiosemicarbazides as Building Blocks for Synthesis of Azoles andAzines (A Review) Sayed M. Riyadh , Shojaa Abed El-Motairi and Anwar A. Deawaly[ HTML Full Text] [ Abstract ] [PDF] [ XML]

DOI : http://dx.doi.org/10.13005/ojc/340201

Methods for the Preparation of Modified Polyorganosiloxanes (A Review)Kostyukovich Alexander Yur’evich , Drozdov Fedor Valer’evich , Vitaly Sergeevich Ivanov , Anton Sergeevich Yegorov andVladimir Viktorovich Men'shikov

[ HTML Full Text] [ Abstract ] [PDF] [ XML]


Diethyldithiocarbamate Doped Graphene Quantum Dots Based Metal Complex Nanoparticles byResonance Light Scattering for Green Detection of Lead(II) – (A Review)Chayanee Kaewprom , Prawit Nuengmatcha and Saksit Chanthai[ HTML Full Text] [ Abstract ] [PDF] [ XML]


Laccase Biosensor: Green Technique for Quantification of Phenols in Wastewater (A Review)Yashas S. R , Shivakumara B. P, Udayashankara T. H and Krishna B. M.[ HTML Full Text] [ Abstract ] [PDF] [ XML]


Nigella Sativa L. Seeds Biomass as A Potential Sorbent of Lead from Aqueous Solutions and WastewatersAbdelhamid Addala , Noureddine Belattar and Maria Elektorowicz[ HTML Full Text] [ Abstract ] [PDF] [ XML]


Gas Sensor with Reduced Humidity Response Based on Metal Oxide Nanoparticles Synthesized by SparkDischargeAlexey Vasiliev , Andrey Varfolomeev , Ivan Volkov , Pavel Arsenov , Alexey Efimov , Victor Ivanov , Alexander Pislyakov ,Alexander Lagutin and Thomas Maeder[ HTML Full Text] [ Abstract ] [PDF] [ XML]


A New Edition of Web of Science

CNKI Scholar (China National Knowledge Infrastructure)

Journal Archived in:

Life Fellowship Awards in

Chemistry by Researchers Societyof Chemical Sciences, Bhopal,

India.

Membership Form of Researchers

Society of Chemical Sciences Email: [email protected]

Click here for RSCS Details

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10/6/2020 Editorial Board : Oriental Journal of Chemistry

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ISSN : 0970 - 020X, ONLINE ISSN : 2231-5039

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Prof.(Dr.) S.A. [email protected]. Iqbal at present is serving as Ex-Director in Crescent College of Technology, affiliated to Rajiv GandhiTechnical University, Bhopal India. He is serving Oriental Journal of Chemistry as Chief Editor since last thirty years. Dr. Iqbal is conducting research on environmental, co-ordination and drug chemistry and hasa credit of producing 26 Ph.D. (s) Dr. Iqbal has published about 120 research papers in internationaljournals and is the author and co-author of 25 books on various topics of chemistry. He has presented hisresearch work in many International Conferences’ and is the reviewer of Elsevier publications and is thevisiting scientist of Japan and Saudi Arabia.

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Prof. Marek WesolowskiMedical University of Gdansk,Department of Analytical Chemistry,Gdansk [email protected] ID: 7006285037

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Dr. Soumyakanti AdhikariBhabha Atomic Research Centre, Mumbai,[email protected] ID: 8441713100

Prof. Dr. Mohamad J. Al-JebooriDepartment of Chemistry, College ofEducation for Pure Science University ofBaghdad. [email protected] ID: 24553673600

Dr Ayssar NahléDepartment of Chemistry, College ofSciences, University of Sharjah,Sharjah, United Arab [email protected] ID: 6603539686

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ORIENTAL JOURNAL OF CHEMISTRY

www.orientjchem.org

An International Open Free Access, Peer Reviewed Research Journal

ISSN: 0970-020 XCODEN: OJCHEG

2018, Vol. 34, No.(2):Pg. 875-880

This is an Open Access article licensed under a Creative Commons Attribution-NonCommercial-ShareAlike4.0 International License (https://creativecommons.org/licenses/by-nc-sa/4.0/ ), which permits unrestrictedNonCommercial use, distribution and reproduction in any medium, provided the original work is properly cited.

Phytosterol Screening of Skin and Seed Extracts ofWild Grape Ampelocissus martinii Planch

WILAIWAN SIMCHUER and PRASONG SRIHANAM*

Creative Chemistry and Innovation Research Unit, the Center of Excellence in Chemistry, Department of Chemistry, Faculty of Science, Mahasarakham University, Kantarawichai,

Maha Sarakham 44150, Thailand.*Corresponding author E-mail: [email protected]


(Received: October 29, 2017; Accepted: January 05, 2018)

ABSTRACT

Reports on phytosterol in wild grape, Ampelocissus martinii Planch fruits are rarelyavailable world wide. We have investigated the total triterpenoid content (TTC) and total sterolcontent (TSC) in skin and seed extracts from different growth stages of wild grape fruits using aspectrophotometric assay. In addition, we analyzed some free sterols using high performanceliquid chromatography (HPLC). The mature fruit showed the highest content of TTC in both theskin and seed extracts. The TSC content was found the highest from skin extract in the ripe stage.The two most common phytosterols found were stig masterol and β-sitosterol. The stig masterolcontent was found the highest in the skin extract of the immature, while β-sitosterol was found inthe seed extract of the ripe fruits. This work indicated that the skin and seed of wild grape fruitsmight be new sources of phytosterol.

Keywords: Wild grape, Phytochemical, Phytosterol, Spectrophotometric assay.

INTRODUCTION

Phytochemicals are secondary metabolitesthat are non-nutritive, naturally occurring, andbiologically active compounds and found in theplant kingdom1. Phytochemicals enrich thebiological activity potential, including anti-inflammation, anti-cancer, antimicrobial, andantioxidant. There are more than a thousand knownphytochemicals2. Phytosterols are one group of

triterpenoid and pervasive in plants. Generally, theirstructures look like to cholesterol, but side chainhas differed in the alkyl position. Among morethan 200 different compounds of phytosterol,β-sitosterol, stigmasterol, and campesterol arepredominate types in higher plants and human diets.The several of vegetable oil, nuts, fruit, berries,grapes, and cereals are important sources of theplant sterols. Wild grape is a potent source ofantioxidants and anti-bacterials from their

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2018, Vol. 34, No.(2):Pg. 881-886


Carbon–Carbon Bond Formation Reaction withPd/reduced Graphene Oxide Composite

PADMAKAR ANANT KULKARNI, SURESH SHAMRAO SHENDAGE*and ASHOK GANUJI AWALE

Department of Chemistry, KET’S Vinayak Ganesh Vaze College of Arts,Science and Commerce Mithagar Road, Mulund (E) Mumbai-400081, India.

*Corresponding author E-mail: [email protected]


(Received: December 03, 2017; Accepted: February 01, 2018)

ABSTRACT

Palladium nanoparticles supported on reduced graphene oxide (Pd/rGO) catalyst wasprepared by using alovera extract in sunlight. The catalyst (Pd/rGO) was employed for the Suzukicross coupling reactions. The characterization of Pd/rGO was done by scanning electronmicroscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction analysis (XRD).The average particle size of Pd was found to be 7±2 nm. The compound showed excellentcatalytic activity with good recyclability for C-C cross coupling reactions.

Keywords: Solar energy, Alo vera, Heterogeneous catalysis, Greener synthesis,Palladium nanoparticles, Reduced graphene oxide, Cross coupling reactions.

INTRODUCTION

In last decades Suzuki–Miyaura cross-coupling reaction has gained considerable attentionbecause of its use in making active pharmaceuticalingredients, agrochemicals, polymers, bioinorganicmaterials and natural products on a laboratory aswell as industrial scale1. In 1981 the first methodwas reported for the preparation of biaryls via C-Ccross-coupling reaction2. In general, homogeneouspalladium complexes are used as catalysts in theSuzuki reaction3.

The reported homogeneous catalysts arefound to have greater catalytic properties thanheterogeneous catalysts in the formation of C-Ccoupling reactions4-6. The several researchersfocused on the development of palladiumcomplexes which efficiently catalyze the reaction7.

The palladium complexes usually showgreater catalytic activity. The main drawbacks ofthese catalysts are availability, stability, recovery,and high cost in addition to their sensitivity toair and moisture. So reactions catalyzed by

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Oriental Journal of ChemistryScopus coverage years: 1989, from 2008 to 2018

Publisher: Scientific PublishersISSN: 0970-020X E-ISSN: 2231-5039Subject area: Chemistry: General Chemistry Pharmacology, Toxicology and Pharmaceutics: Drug Discovery

Environmental Science: Environmental Chemistry Biochemistry, Genetics and Molecular Biology: Biochemistry

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Microstructure characterization of natural magnetite from sand marinabeach by high energy milling (Article) (Open Access)

, , ,

Department of Chemistry, Diponegoro University, Semarang, Central of Java, 50275, Indonesia

AbstractIn this work, we performed an experimental investigation the change of microstructure of magnetite by high energy milling -3D (HEM-3D) method using planetary ball milling at 400 rpm speed. The present studies mainly

focusses on the effect of milling on crystallinity and phase of magnetite by XRD, particle size by PSA and themorphology by SEM. The increasing of the ball mass in the milling process, mass ratio magnetite : ball (P/B) 1: 1, 1:3 and 1: 5 give the magnetite particles smaller (< 1μm), the crystallinity decreases but the peaks at (2 2 0), (3 1 1), (4 00), (5 1 1), and (4 4 0) were keep appearing. This shows that the phase of cubic spinel does not change. Rising the milling time for 1 h, 3 h and 5 h can lead to decreasing of size and crystallinity. Even milling time for 5 h on mass

ratio of magnetite : ball (P/B) 1: 5 causes the magnetite phase to change to amorphous. © 2018 Oriental ScientificPublishing Company. All rights reserved.

SciVal Topic Prominence

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Author keywordsHigh energy milling -3D. Microstructure Natural magnetite Sand marina beach

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Universitas Diponegoro UNDIP

Funding text

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Oriental Journal of ChemistryVolume 34, Issue 2, 2018, Pages 868-874

Sriatun Darmawan, A. Sriyanti Cahyani, W.

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Titanomagnetite | Ilmenite | Carbothermal Reduction

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Optimization of the high energyball-milling: Modeling andparametric study

Ghayour, H. Abdellahi, M.Bahmanpour, M.

A comparative study of physicalproperties in Fe3O4nanoparticles prepared bycoprecipitation and citratemethods

Gholizadeh, A.

Controlled synthesis of water-dispersible andsuperparamagnetic Fe3O4nanomaterials by a microwave-assisted solvothermal method:From nanocrystals tonanoclusters

Jing, X. Liu, T. Wang, D.

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References (16)

Sriatun, Adi Darmawan and Sriyanti, gratefully acknowledge financial support from of Besides APBN DPA SUKPALPPM Diponegoro University, and Department of Chemistry for the facilities to carry out this research.

Nugraha, P.A., Sari, S.P., Hidayati, W.N., Dewi, C.R., Kusuma, D.Y. (2016) AIP Conference Proceedings, 1, pp. 17-47.

Shpotyuk, O., Bujňáková, Z., Sayagués, M.J., Baláž, P., Ingram, A., Shpotyuk, Y., Demchenko, P.

(2017) Materials Characterization, 132, pp. 303-311. . doi: 10.1016/j.matchar.2017.08.028

Gong, J.-L., Wang, B., Zeng, G.-M., Yang, C.-P., Niu, C.-G., Niu, Q.-Y., Zhou, W.-J., (...), Liang, Y.

(2009) Journal of Hazardous Materials, 164 (2-3), pp. 1517-1522. . doi: 10.1016/j.jhazmat.2008.09.072

Hui, C., Shen, C., Yang, T., Bao, L., Tian, J., Ding, H., Li, C., (...), Gao, H.-J.

(2008) Journal of Physical Chemistry C, 112 (30), pp. 11336-11339. . doi: 10.1021/jp801632p

Klotz, S., Steinle-Neumann, G., Strässle, Th., Philippe, J., Hansen, Th., Wenzel, M.J.

(2008) Physical Review B - Condensed Matter and Materials Physics, 77 (1), art. no. 012411. .

doi: 10.1103/PhysRevB.77.012411

Marinca, T., Chicina, H., Neamu, B., Popa, F., Isnard, O., Chicina, I. (2015) Studia Universitatis Babes-Bolyai Physica, 1, p. 60.

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ISSN 0970020X, 22315039

Coverage 1989, 2008-2018

Scope Oriental Journal of Chemistry was started in 1985 with the aim to promote chemistry research. The journal consists ofarticles which are rigorously peer-reviewed. The journal was indexed in Emerging Science citation index in 2016. TheEditorial board member consists of eminent international scientist in all �elds of Chemistry. Details of each memberand their contact information is mentioned in website. The journal has thorough ethics policies and uses plagiarismdetection software(ithenticate) to screen each submission. The journal has recently partnered with publons as a partof making our reviews more transparent. The journal has recently incorporated PlumX for article level matrix. Thejournal is promoting research on all social and academic platforms mentioned in PlumX guidelines. The journal usesgoogle maps to improve on the geographical distribution of Editorial board members as well as authors.

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Quartiles

The set of journals have been ranked according to their SJR and divided into four equal groups, four quartiles. Q1 (green)comprises the quarter of the journals with the highest values, Q2 (yellow) the second highest values, Q3 (orange) the thirdhighest values and Q4 (red) the lowest values.

Category Year QuartileBiochemistry 2009 Q4Biochemistry 2010 Q4Biochemistry 2011 Q4Biochemistry 2012 Q4

SJR

The SJR is a size-independent prestige indicator thatranks journals by their 'average prestige per article'. It isbased on the idea that 'all citations are not createdequal'. SJR is a measure of scienti�c in�uence ofjournals that accounts for both the number of citationsreceived by a journal and the importance or prestige ofthe journals where such citations come from Itmeasures the scienti�c in�uence of the average articlein a journal it expresses how central to the global

Citations per document

This indicator counts the number of citations received bydocuments from a journal and divides them by the totalnumber of documents published in that journal. Thechart shows the evolution of the average number oftimes documents published in a journal in the past two,three and four years have been cited in the current year.The two years line is equivalent to journal impact factor™ (Thomson Reuters) metric.

Cites per document Year ValueCites / Doc. (4 years) 2008 0.000Cites / Doc. (4 years) 2009 0.095Cites / Doc. (4 years) 2010 0.189Cites / Doc. (4 years) 2011 0.165Cites / Doc. (4 years) 2012 0.416Cites / Doc. (4 years) 2013 0.497Cites / Doc. (4 years) 2014 0.457Cites / Doc. (4 years) 2015 0.472Cites / Doc. (4 years) 2016 0.608Cites / Doc. (4 years) 2017 0.612

Total Cites Self-Cites

Evolution of the total number of citations and journal'sself-citations received by a journal's publisheddocuments during the three previous years.Journal Self-citation is de�ned as the number of citationfrom a journal citing article to articles published by thesame journal.

Cites Year ValueS lf Cit 2008 0

External Cites per Doc Cites per Doc

Evolution of the number of total citation per documentand external citation per document (i.e. journal self-citations removed) received by a journal's publisheddocuments during the three previous years. External

% International Collaboration

International Collaboration accounts for the articles thathave been produced by researchers from severalcountries. The chart shows the ratio of a journal's

2009 2010 2011 2012 2013 2014 2015 2016 2017 2018 2019

Biochemistry

Chemistry (miscellaneous)

Drug Discovery

Environmental Chemistry

2009 2011 2013 2015 2017 2019

0.075

0.15

0.225

0.3

Cites / Doc. (4 years)Cites / Doc. (3 years)Cites / Doc. (2 years)

2008 2010 2012 2014 2016 2018

0

0.2

0.4

0.6

0.8

2008 2010 2012 2014 2016 2018

0

400

800

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2018, Vol. 34, No.(2):Pg. 868-874


Microstructure Characterization of Natural Magnetite from Sand Marina Beach by High Energy Milling

SRIATUN1*, A. DARMAWAN1, SRIYANTI1 and W. CAHYANI1

1Department of Chemistry, Diponegoro University, Semarang 50275, Central of Java, Indonesia.*Corresponding author E-mail: [email protected]


(Received: December 18, 2017; Accepted: January 25, 2018)

ABSTRACT

In this work, we performed an experimental investigation the change of microstructure ofmagnetite by high energy milling-3D (HEM-3D) method using planetary ball milling at 400 rpmspeed. The present studies mainly focusses on the effect of milling on crystallinity and phase ofmagnetite by XRD, particle size by PSA and the morphology by SEM. The increasing of the ballmass in the milling process, mass ratio magnetite: ball (P/B) 1: 1, 1: 3 and 1: 5 give the magnetiteparticles smaller (< 1μm), the crystallinity decreases but the peaks at (2 2 0), (3 1 1), (4 0 0),(5 1 1), and (4 4 0) were keep appearing. This shows that the phase of cubic spinel does notchange. Rising the milling time for 1 h, 3 h and 5 h can lead to decreasing of size and crystallinity.Even milling time for 5 h on mass ratio of magnetite: ball (P/B) 1: 5 causes the magnetite phase tochange to amorphous.

Keywords: Microstructure, Natural magnetite, Sand marina beach, High energy milling-3D.

INTRODUCTION

Iron sand occurs naturally in severalregions throughout the world. Iron sand is one ofIndonesia’s natural mineral resources, which isspread over the islands along the coast of JavaIsland, Kalimantan and Sumatra. Iron sand is aspecial type of sand that’s rich in the metal iron, thecolor is dark gray or black, consisting of (Fe) iron asa major element and a small amount of Ti, Si, Ca,

Mn and Vanadium. They provide a raw material ofrelatively low grade, whereas in the southern coastof Yogyakarta containing 5.85 % to 95.11% of iron.

In addition to magnetite in iron sand also containsother minerals such as rutile, ilmenite and hematite1.While most sand contains at least some trace of

iron, therefore it has a distinct dark-gray or blackcolor, which is in stark contrast to the white-yellowcolor of regular sand.

869SRIATUN et al., Orient. J. Chem., Vol. 34(2), 868-874 (2018)

Iron sand is a magnetic material that iswidely used in various fields such as electronics,energy, chemistry, ferrofluidics, catalysts, andmedical diagnostics2. The application of iron sandwas inseparable from the development of studiesof nanomaterials demanding that they be in theorder of nanometers. Magnetite or Fe3O4 is one ofthe iron oxide phases which has the greatestmagnetic or ferromagnetic properties among theother phases. Iron oxide has four phases, namelymagnetite (Fe3O4), maghemite (γ-Fe2O3), hematite(α-Fe2O3), and geotite (FeO(OH)). Only magnetiteand maghemite have magnetic properties3.

Magnetite (Fe3O4) is known as a class ofiron oxide compound with a cubic inverse spinelstructure and has face centered cubic close packedoxygen anions and Fe cations occupying interstitialtetrahedral and octahedral sites4,5. Nano-sizedmagnetite particles provide many advantages suchas for the separation of magnetic contaminants inwater, large of surface area and the ability to bindthrough electro-chemical interactions to form sludge.It is also applied to drug delivery and magneticresonance technology and others.

For the synthesis of nanosized magnetiteparticles can be synthesized through variousmethods such as mechanical milling6,sol-gels, direct decomposition7, co-precipitation8,microwave-heating9 and solvothermal10,11.Mechanical milling method is one way to reducethe magnetite size is the cheapest and easy.Mechanical milling is defined as the mechanicalbreakdown of magnetite into smaller withoutchanging their state of aggregation. The methodwas used to increase the surface area and inducedefects which is needed for subsequent operationssuch as chemical reactions, sorption. Milling alsoto increase the proportion of regions of high activityin the surface12.

Furthermore, this research the small sizeof magnetite from iron sand was prepared bymechanical milling method using high energyplanetary ball mill. Kinetic energy of the ballsdepends not only on its velocity, but also on its massand how long the collision occurred, due to in thiswork investigated the ratio of magnetite and ballmass in the planetary ball mill and the time of impactduring collision.

MATERIALS AND METHODS

MaterialsIron sand was taken from Marina Beach in

Semarang.

InstrumentationsMagnet permanent, High energy planetary

ball mill-3D, X-ray diffraction (XRD) RigakuMultiplex with Cu Ká radiation (λ = 1.54184 Ao) atgenerator voltage 40 kV and current 40 mA, ParticleSize Analyzer (PSA) Horiba SZ-100, Scanningelectron microscope (SEM) JEOL JED 2300.

ProcedureMagnetite preparation

The natural iron sand from Marina BeachSemarang cleaned and washed using aquadest,dried in oven at 80 oC for 24 hours. Naturalmagnetite was extracted from natural iron sandusing permanent magnet until 12 times. Thistreatment produces powder material darkgray-black color. Refinement of magnetite particlescarried out by mechanical milling method using highenergy planetary ball mill (HEM-E3D) instrument.The milling was done on mass ratio of magnetite:ball (P/B) 1:1, 1:3 and 1:5, speed 400 rpm. Milling ofmagnetite carried out for 1, 3 and 5 hours. Milledmagnetite dried at 150 oC for 1.5 hours. Finally, themicrostructure characterization of product was doneby X-ray diffraction (XRD) to find out the structure ofmagnetite crystals, PSA to determine the size ofmagnetite particle, SEM to know the surfacemorphology.

RESULTS AND DISCUSSIONS

In this work the change of crystal structure,particle size and morphology of magnetite wasinvestigated. The method is high energy milling(HEM) used planetary ball mill. The choice of thismethod due to it can reduce the material up to thenano order (nano particle) inside a relatively shorttime under conditions atmosphere at roomtemperature during process milling. This methodusing energy collision between the crushing ballsand chamber walls are rotated and driven in acertain way. The change of crystal structure, particlesize and morphology of magnetite was studied onvariation the mass ratio magnetite:ball (P/B 1:1, 1:3and 1:5) and milling time (1, 3 and 5 hours).

870 SRIATUN et al., Orient. J. Chem., Vol. 34(2), 868-874 (2018)

Physical changes of magnetiteThe process of separation of magnetite

compounds from iron sand is done repeatedly, it isintended that the compound to be obtained has ahigh purity. The separation process with magnetsalso uses a certain distance, the farther the magnetis closer to the iron sands, the less iron oxideattaches. This makes the sample (magnetite) higherpurity and less impurities, although there is still thepossibility of the other oxide compounds sticked toa permanent magnet. The Fig. 1 following is theembodiment of magnetite extracted from iron sand.

after mechanical milling becomes smaller and softerthan the separated iron sand. This is the advantagesof mechanical milling method that ball mill is notsensitive to metal. The superiority of high energymilling is able to produce smaller particles in shortermilling time12.

Crystal structure of magnetiteBased on the results of the analysis using

X-ray diffraction on magnetite powder before millingtreatment with HEM-3D obtained X-ray diffractionpattern as shown in Fig. 3. There are five highestpeaks at 2è angle of 30.09o; 35.46o; 43.09o; 56.98o;and 62.59o. Furthermore the highest peaks werecompared with Joint Committee of PowderDiffraction Standard (JCPDS) number 89-4319 withthe highest peaks at 2θ angle of 30.083o; 35.434o;43.064o; 56.949o; and 62.536o. Based on dataobtained from XRD, the compound is magnetite.

Fig. 1. The original iron sand from marina beachbefore extraction treatment with permanent

magnet (A) Magnetite after extraction treatment

(a) (b)

The extracted iron sand powder thenperformed mechanical milling with severalvariations of the mass ratio of magnetite:ball (P/B)1:1, 1:3 and 1:5 for 1, 3 and 5 h at speed 400 rpm.Magnetite obtained from the milling results has asofter texture and dark black as shown in Figure 2.

Fig. 2. Milled magnetite

It is clearly from Fig. 1A and 1B and Fig. 2,the difference in color and size of iron sand. In ironsand that has been separated with permanentmagnet looks blacker than iron sand that has notbeen separated. This is due to the reduction ofimpurities from the iron sand so that the iron sandlook blacker after extraction using permanentmagnet as much 12 times. This shows that theseparation of iron sand from impurity elements bythis method more effectively. The size of iron sand

Data of X-ray diffraction on magnetite afterHEM-3D treatment with mass ratio of magnetite:ball (P/B) 1: 1, 1: 3 and 1: 5 and time collision 1, 3and 5 h showed in Fig. 4, Fig.5 and Fig. 6. Alldiffraction peaks correspond to the peak diffractionat (2 2 0), (3 1 1), (4 0 0), (5 1 1), and (4 4 0). Of thehighest peaks are compared with the JointCommittee of Powder Diffraction Standard (JCPDS)number. 79-0418 shows indexed to the Fe3O4 cubicspinel phase.

The XRD datas show that in all P / B ratio1, 1: 1: 3 or 1: 5 with milling process for 1 and 3 hstill indicates conformity with reference magnetite.When the milling for 5 h is only in P/B 1: 1 and P/B1: 3 which still shows the suitability and even this isonly at the peak of 2´ = 35.92o and 63.02o at P/B 1:1 and 36.19o and 63.15o at P/B 1: 3, where the peakof the diffractogram is very low, whereas in P/B 1: 5there is no correspondence with the reference

Fig. 3. Diffractogram XRD of magnetite afterextraction treatment


magnetite. This suggests that long-term millingtreatments and strong collisions (heavier ball) cansignificantly reduce magnetic particle size, thesetreatments also decreased degrade of crystallinity.The increasing of ball to magnetite mass ratio(heavier ball) would enhancing the kinetic energyduring milling. Based on kinetic energy equation:

in which is the kinetic energy, m and v arerespectively the mass and velocity of the balls. Inthis research the velocity was constant.

When the colliding ball mass is heavier,so the kinetic energy increases. The high of kineticenergy would cause the particles to collide with eachother, where this would decrease in particle size.

Fig. 5. Diffractogram milled magnetite by mass ratio of magnetite:ball (P/B) 1:3




This is in accordance with data that hasbeen revealed by previous research. It was reportedthat the enhancing energy during milling, resultedby the increase of ball to powder weight ratio (BPR)and vial speed not only can accelerate theformation of the products but also changes theresultant phases4. The balls play an important rolein its efficiency so that a small change in type,shape, weight or mass and size distribution of theballs can dramatically affect the milling process5.The increase of the number of balls at high BPRratio, has a quite negative effect on the millingperformance6.

Particle size of magnetiteThis matter proves that the milling process

is done to magnetite powder can causing thedestruction of the grains magnetite powder as aresult collision between magnetite powder andmilling balls. To know more clearly destruction of

graphite powder during process milling, then themeasurement magnetite particles by particle sizeanalyzer (PSA) instrument. The choice of particlemeasurement methods of nanoscale and micro sizeis usually by using a wet method PSA (particle sizeanalyzer) method, because it is an accurate methodwhen compared to other methods. Small particleshave a tendency for high agglomeration, the choiceof wet method on PSA because the particles aredispersed into the medium so that the particles donot agglomerate (clump). Therefore the measuredparticle size is the size of a single particle andprovides overall information on sample conditions.

Distribution particle size test by particlesize analyzer (PSA) aims to determine particle sizedistribution after mechanical milling process byHEM-3D for 1 h, 3 h and 5 hours. The result ofmilled magnetite can be seen in Figure 7.

Fig. 7. Graph of magnetite size distribution on mass ratio magnetite: ball(P/B) 1: 1 (A); 1: 3 (B) and 1: 5 (C)


In Fig. 7 it is observed that the magnetite/ball mass ratio (P/B) of 1: 1 increase in time causesa significant reduction in particle size. When for 1 hmilling the size range varies as well as for 3 h,however the milling is performed for 5 h gives impactto a more homogeneous magnetite size (the peakis not widened). Significant reduction in sizeoccurred in treatment with a mass ratio of P/B 1: 3and 1: 5. This is due to the heavier the ball and thelength of time the greater the energy given to collidewith the magnetite particles. Thus the magnetitetreatment with HEM (high energy milling) is effectiveenough to reduce the size to less than 1000 nm(<1μm).

Morphology of magnetiteThe surface morphology of a material can

be observed using Scanning Electron Microscope.The basic principle of work on SEM is the nature ofelectron waves, it is diffraction at very small angles.Electrons are dissipated by a charged sample. Theimage formation on SEM comes from the electronbeam reflected by the sample surface. If the sampleused is not conductive, the sample must first becoated with gold16.

Based on the SEM image in Fig. 8, theaddition of spherical periods has an effect on thereduction of natural magnetite particle size. In theP/B ratio 1: 1 the particle size varies from small tolarge size. When the mass of balls increase 3 timesto magnetite (P/B 1: 3), the collision between themagnetite and the ball gets stronger or the greaterthe energy that causes the breaking of the particlesto become smaller and appear more homogeneous.In addition to the ball up to 5 times the magnetiteperiod (P/B 1: 5) the particles also become smallerbut the possibility of agglomeration appears to belarger if compared to P/B 1: 3. The size of themagnetite particles is slightly affected by the lengthof time the collision with the ball on the planetaryball mill. The milling process for 1 to 3 hours givesalmost the same result, observed on surfacemorphology at P/B 1: 1 for 1 h is almost equal to 3hours. Similarly to P/B 1: 3 for 1 hour is almost thesame as for 3 hours, and P/B 1: 5 for 1 hour with 3hours. However, when the milling for 5 h on thethree variations of the ball period gives significantlydifferent results with the previous. This is especiallyobserved in P/B 1: 3 for 5 hours, visible particleshaving clear and firm shape and cleaner than others.

P/B 1:1 1h P/B 1:1 3h P/B 1:1 5h

P/B 1:3 1h P/B 1:3 3h P/B 1:3 5h

P/B 1:5 1h P/B 1:5 3h P/B 1:5 5h

Initial Magnetite

Fig. 8. Morphology of milled magnetite and initial magnetite bymagnification 5000x


CONCLUSION

From the results and discussion can beconcluded that the HEM-3D treatment with 400 rpmspeed can reduce particle size and increase theuniformity of shape and magnetite size. Theincreasing of the ball mass in the milling process,this means in the mass ratio of magnetite:ball (P/B)1: 1, 1: 3 and 1: 5 give the magnetite particles smaller,the crystallinity decreases but the phase does notchange. Rising the milling time can lead todecreasing of size and crystallinity. Even milling

time for 5 h on mass ratio of magnetite: ball (P/B) 1:5 causes the magnetite phase to change to

amorphous

ACKNOWLEDGEMENT

Sriatun, Adi Darmawan and Sriyanti,gratefully acknowledge financial support from of

Besides APBN DPA SUKPA LPPM DiponegoroUniversity, and Department of Chemistry for thefacilities to carry out this research.

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2. Shpotyuk, O.; Bujòáková, Z.; Sayagués, M.J.;Balá•, P.; Ingram, A.; Ya.Shpotyuk,Demchenko, P. Materials Characterization.,2017, 132, 303-311.

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4. Hui, C.; Shen, C.; Yang, T.; Bao, L.; Tian, J.;Ding, H.; Li, C.; Gao, H.J. J. Phys. Chem. C.,2008, 112, 11336-11339.

5. Klotz, S.; Steinle-Neumann, G.; Strassle, T.;Philippe, J.; Hansen, T.; Wenzel, M.J. Phys.Rev. B., 2008, 77, 12411-1-1241-4.

6. Marinca, T.; Chicinaˆ, H.; Neamˆu, B.; Popa,F.; Isnard, O.; Chicinaˆ, I. Studia UniversitatisBabes-Bolyai, Physica., 2015, 1, 60.

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S. Bull Mat Sci., 2005, 28, 115-119.

Microstructure Characterizationof Natural Magnetite from SandMarina Beach by High Energy

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