SYNTHESIS MAGNETITE AND CHARACTERIZATION WITH FTIR, PSA AND

MAGNETITE EXTERNAL

1. INTRODUCTION
1.1. Objectives
To study the process sintesis megnetit used low energy and characterization compound which
produce with FTIR
1.2. Basic Theory

Magnetite nanoparticles are a group of iron oxides that have some typical properties such as:
very small particle size, large surface area and effective in transferring mass [ CITATION
NIA13 \l 1057 ]. Nanoparticle of magnetite have some kind such as γ-Fe2O3, α-Fe2O3, dan
Fe3O4. Each of that particle kind have different characteristic. like γ-Fe2O3 that have cubic
closed-packed structure with good chemistry equilibrium, and usually used for recorder with
magnet. α-Fe2O3 have rhombohedral structure, this kind is that most stable but have anti-
ferromagnetik character under temperature Neel (< 955 K). while Fe3O4 magnetit have spinel
structure rolled back at suhu kamar (Muh Pauzan. et al., 2013).
Naturally these materials are found in the form of iron oxide Minerals such as magnetit
(Fe3O4), maghemit (γ-Fe2O3) and hematit (α-Fe2O3). Based on the advantages of magnetism,
the Iron oxide material has been exploited widely for various products such as sensor, tinta,
katalis, thin film and some product have tech nanoparticle. (Mahardika PrasetyaAji. et al.,
2007).
hence contains two iron spesies that are ferro (tereduksi) and feri (teroksidasi), magnetite is
often called iron (II) (III) oxide (Blaney in Jumaeri, et al., 2018 ). The crystal structure from
third Iron oxide can described in the form field of packaging tight anion oxygen with Iron
cations in octahedral site atau tetrahedral. In magnetite the ions of oxygen is in forming cubic
close-packed. Magnetite have spinel structure backward with Fe(III) ions distributed randomly
between oktahedral Sie and tetrahedral and Fe(II) ions in the octahedral site. (Jumaeri, et al.,
2018)
Magnetite is a type of iron oxide with Fe3O4 chemical formula. The color of particle is and
ferimagnetic with highest value magnetization amount 92 emu/g. Synthesis magnetite has been
developed with various methods, such as kopresipitasi, sol-gel, hidrotermal, dan
electrochemistry[ CITATION Ret17 \l 1057 ].
kopresipitasi Method is once synthesis method inorganic compound that based in precipited
More then one substance secara bersama-sama when melewati titik jenuhnya. Kelebihan lain
from kopresipitasi method is used suhu kamar and easy to mengontrol particle size so the time
needed relative more short[ CITATION Sur15 \l 1057 ].
Nanopratikel have as a base Fe3O4 has been widely used in imobilisation and separation
protein atau enzyme. Selain itu also used to be lost the catalyst, and toxic elements from
 industry waste while nanomagnetic film widely used in Electric device and electronic, sensor,
digital storage that have high kerapatan, and protect electromagnetic. Selain itu magnetite film
also has been many dipelajari and diterapkan in tumor hyperthermia as intermediatery that
guide the magnet field to melokalisasikan terapi radioaktif and obat-obatan[ CITATION
Sur15 \l 1057 ].
Spektrofotometri Infra Red atau Infra Merah merupakan suatu metode yang mengamati
interaksi molekul dengan radiasi elektromagnetik yang berada pada daerah panjang gelombang
0,75 – 1.000 µm atau pada Bilangan Gelombang 13.000 – 10 cm -1. Berdasarkan pembagian
daerah panjang gelombang, sinar infra merah dibagi atas tiga daerah: daerah infra merah dekat,
daerah infra merah pertengahan, daerah infra merah jauh. Daerah panjang gelombang yang
digunakan pada alat spektrofotometer infra merah adalah pada daerah infra merah pertengahan,
yaitu pada panjang gelombang 2,5 – 50 µm. Interaksi antara sinar infra merah dengan molekul
hanya menyebabkan vibrasi, yaitu bergerak pada tempatnya. Vibrasi molekul sangat khas untuk
suatu molekul tertentu dan biasanya disebut finger print. Daerah antara 4000 – 2000 cm-
1
merupakan daerah yang berguna untuk identifkasi gugus fungsional Energi yang dimiliki oleh
sinar infra merah hanya cukup kuat untuk mengadakan perubahan vibrasi (Ardhiana. et al.,
2014).

2. EXPERIMENT METHOD
2.1. Apparatus and reagent

Apparatus : Reagents :

1. Beaker glass 50 ml 1. FeSO4.7H2O

2. Measure glass 10 ml 2. FeCl3.6H2O
3. Volumetric flask 10 ml 3. NaOH
4. stirer 4. KBr
5. Hot plate 5. Aquades
6. Neraca Analitik
7. Indikator universal
8. Funnel
9. Watch glasses
10. Oven
11. Desikator
12. Ultrasonic probe
13. Filter paper

2.2. Skema
Synthesis Magnetit Fe3O4 with mekanik (low energy)

Weight 1,3 g (0,005 mole) Each of compound dissolve in

FeSO4.7H2O and 2,7 g 10 ml aquabides.
(0,010 mole) FeCl
Add NaOH 3.6H1,5
solution 2O M
And then mixed both solution and
at 50º C and still stir until
put down in magnetit stirer Hot plate
pH = 12
 Next, the filtered precipitate with Drying the precipitate at
filter paper and washed until pH 100º C during 1 hour
netral
Characterization Magnetit (with FTIR)

Take the cable, turn on the And then fill the sample table,
machine in behind, open the click background, wait to
spectrum application (double scanning background 100%
click) and then put the sample

And the other sample check

the characteristic magnetic Cleanse all of device with acetone
with external magnetic
Characterization with PSA
Added the sample in kuvet,
Turn on the adaptor, setting temperature etc. Put the
machine, and CPU computer sample in PSA machine
(wait). Prepare sample with
plastic kuvet/ kuarsa

And the last turn off the machine,

when we turn off the machine so
reverse from trun on the machine
(CPU computer, machine,
andadaptor)
2.3. Procedure

Procedure Observation
1. Make the solution FeSO4.7H2O
a. Weight 1,3 g 0,005 mol The mass of FeSO4.7H2O = 1,4012 grams
FeSO4.7H2O
The volume of aquades = 10 ml
The colour of solution = merah bata
b. Dissolve FeSO4.7H2O with
The colour of precipitate = -
aquades
The mass of FeCl3.6H2O = 2,7048 grams

The volume of aquades = 10 ml

c. Weight 2,7 g FeCl3.6H2O The colour of solution = coklat tua
The colour of precipitate =
d. Dissolve FeCl3.6H2O with aquades
2. Mix the solution FeSO.4H2O and
 FeCl3.6H2O
a. FeSO4.7H2O
Before rx After rx
Colour Merah bata Orange
kecoklatan
b. FeCl3.6H2O Precipitate - -

Before rx After rx
Colour coklat Orange
kecoklatan
Precipitate
3. Add NaOH 1,5 M pH before = 3
pH after = 12
The temperature of NaOH = 50º C
4. Filter and wash the precipitate pH = 7
5. Drain the precipitate The temperature = 100º C
The time = 1 hour
The mass after dry = 2,0134 grams
6. Characterization
a. FTIR Uluran OH, tekukan OH, C-N, C=O,N= O,
Fe-O
b. Magnetit eksternal
(+)
c. PSA (Particle size analysis)

3. RESULT AND DISCUSSION

3.1. Result
 In the first areas between 2500-4000 with wave number X (cm-1) = 3433,77 cm-1 have
gugus fungsi uluran OH
 In the second areas between 2000-1500 with wave number X (cm-1) = 1631,45 cm-1 -
have gugus fungsi tekukan OH
 In the third areas between 1500-1000 with wave number X (cm-1) = 1344,06 cm-1 have
gugus fungsi C-N, in 1113,52 cm-1 have gugus fungsi C=O
 In the fourth areas between 1000-500 with wave number X (cm-1) = 892,42 cm-1 have
gugus fungsi N= O and in 570,66 cm-1 have gugus fungsi Fe-O

 The Rendemen of Magnetite

The mass after drying

X 100%
The mass of FeSO 4 .7 h 2 O+the mass of FeCl 3.6 H 2 O

2,0134
= X 100%
4,1060

= 49,035 %

3.2. Discussion
In this experiment we learn about the process producing magnetit used low energy and
characterization compound that product with FTIR, character from this magnet and distribution
particle size.

The first we producing magnetite from the materials FeSO 4.7H2O 1,4012 grams and FeCl3.6H2O
2,7048 grams. The colour of FeSO 4.7H2O is red brick and the colour of FeCl3.6H2O is dark brown.
After both mixed the colour of solution mixed is orange kecoklatan and in this reaction produce
precipitate, maybe because the once of sample is not good condition.

The reaction is :

FeSO4 (aq) + 2 FeCl3 (aq) + 8NaOH (aq) Fe3O4 (s) + Na2SO4 (aq) + 6NaCl (aq) + 4H2O (l)

And after the both of solution mixed the solution add with drops NaOH solution 1,5 M at
temperature 50º C until pH of solution is 12. pH the solution is 3 before added NaOH. And when
we mixed NaOH solution with the solution mixed the colour is black. Because …. The added
NaOH solution until pH 12 because …… After that filter the solution mixed and wash the
precipitate until the pH of filtrate is netral this is because ….. And then drying the precipitate at
temperature 100º C during 1 hour. And we get the mass of precipiitate is 2,0134 grams.

And afer that we analysis characteristic of magnetite with FTIR device. This analysis to know what
the fungtion group yang contained in megnetite compound. And in experiment the magnetit
compound e contains fungtion group OH in wave number X(cm-1) = 3433,77 and 1631,45, C-N in
wave number X(cm-1) = 1344,06 , C=O in wave number X(cm-1) = 1113,52 , NO three bond in
wave number X(cm-1) = 892,42, and Fe-O in wave number X(cm-1) = 570,66 . The method to know
or determine fungtion group in spektrofotometry infra Red with read spektra FTIR is :

The first you must determine wick X and Y from spectrum. Wick X as wave number and the
amount between from 400-4000, wick Y as percent transmitasi and the amount between from 0-
100.

The second you determine the top characteristic.

The third is determine the area spectrum IR , the area can separation to be four areas. The first area
is from 4000-2500, the second areas from 2500-2000, the third areas from 2000-1500, the fourth
between from 1500-400.

The fourth determine fungsional groups that adsorbs in four areas and identifying the fungtion
group of magnetite.

Spectrofotometry infra Red many more used to identifying compound with fungtion group. In area
1400-4000 cm-1 there is left part of spectrum IR is special area useful to identify fungtion groups,
that is absorbsi from vibrasi ulur. So to identify the fungtion group from a sample attend enough
 from areas 1400 to left. daerah yang berada disebelah kanan bilangan gelombang 1400 cm-1 sering
kali sangat rumit karena pada daerah ini terjadi absorbsi dari vibrasi ulur dan vibrasi tekuk, but
each of organic compound have absorbsi that unique in thi area. This area often called finger print
area. FTIR must saved in moist area because Monokromator IR made from salt NaCl, KBr, CsBr,
or LiF and to prevent damage in the optic instrumentation.

And the next we analysis PSA (particle size analysis) to know the particle size of magnetite. The
objectives for this procedure to gaet nanoparticle from magnetite. but to gaet nanoparticle needed
long times and must use instrument modern. Partikel yang berukuran lebih kecil dari 20 nm akan
cenderung kehilangan sifat magnetisnya sedangkan yang lebih dari 50 nm akan cenderung
mengendap karena pengaruh gaya gravitasi. Diharapkan bahwa produk nanopartikel magnetit yang
dihasilkan memiliki ukuran nanopartikel yang sesuai. Pada analisis PSA ini maka sampel hasil
sintesis magnetite yang sudah dikeringkan akan dihaluskan selama 1 jam untuk mendapatkan
ukuran nanopartikel yang sesuai sehingga ketika dilarutkan akan terdispersi. Setelah sampel
dihaluskan maka sampel dilarutkan dengan asam sitrat dan dimasukkan ke dalam alat sonikator.
Kami mengetahui bahwa ukuran partikel sintesis magnetite dalam ukuran kecil karena setelah
sampel hasil sintesis magnetite dihaluskan kemudian dilarutkan dalam aquades maka dihitung
berapa lama sampel akan mengendap. Ketika sampel mengendap dalam waktu sudah melebihi 1
menit maka partikel sampel tersebut sudah berukuran kecil dan jika sampel lebih cepat mengendap
maka partikel sampel masih berukuran besar. Namun dengan prosedur ini belum bisa kita
mengatakan bahwa sampel sudah dalam keadaan mikro atau nano sebelum di analisis ukurannya
dengan PSA. Dan dalam analisis ini kami hanya mampu mendapatkan magnetite dengan ukuran
mikro partikel karena kurangnya waktu dalam penghalusan sampel hasil sintesis magnetite.

4. QUATIONS AND ANSWER

QUATIONS
a. Explain the formed reaction of magnetite in method upon!
b. Explain which the better result from the mecanic method and ultrasonic method!
c. Explain the basic prinsip of spektrofotometry FTIR and PSA

ANSWER

a. FeSO4 (aq) + 2FeCl3 + 8NaOH (aq) Fe3O4 + NaSO4 (aq) + 6NaCl + 4H2O (l)
b.
c. The basic prinsip of spektrofotometri FTIR
Manfaat : for help know or analysis the bangun formula in a compound.
Prinsip kerja FTIR : pengadsorbsian energi pada berbagai frekuensi di deteksi oleh
spektofotometer IR, yang memplot jumlah radiasi IR yang diteruskan melalui cuplikan
sebagai fungsi dan radian. Plot tersebut disebut spektrum IR.
The basic prinsip of PSA
Prinsip kerja PSA : menentukan ukuran partikel, partikel didispersikan ke media
pendispersi sehingga partikel tidak saling menggumpal.
 5. CLOSING
4.1. Conclusion
Generally spektrofotometer IR used to identifying fungtion group in compound, terutama
senyawa organik. Setiap serapan pada panjang gelombang tertentu menggambarkan adanya
suatu gugus fungsi spesifik.
The rendemen of magnetite is 49,035 %
The magnetite have fungtion group ....... in first area ,...... in second areas,........ in third areas,
and ....... in fourth areas
The magnetite have paramagnetite properties.
4.2. Suggestion

a. Practitioner should first read and understand the lab manual carefully
b. Mutual collaboration between group members
c. Ask the lab assistant or lecturer if there are difficulties
d. Practitioner should measure accurately

6. Reference

Agnestisia, R., 2017. Synthesis & Characterization of Magnetit (Fe3O4) and Its Applications As. Sains
dan Terapan Kimia, 11(2), p. 61.

HANDAYANI, N. W. D., 2013. SYNTHESIS OF MAGNETITE Mg/Al-NO3 HYDROTALCITE

(UMHT) WITH THE ASSISTANCE OF SONOCHEMISTRY METHOD AND ITS APPLICATION
AS ADSORBENT OF [AuCl4]-. Skripsi, p. 3.

Mahardika PrasetyaAji, A. Y. d. S. B., 2007. SINTESIS NANO PARTIKEL MAGNETIT,

MAGHEMIT DAN HEMATIT DARI BAHAN LOKAL. Indonesian Journal ofMaterials Science, p.
106.

Muh Pauzan, T. K. S. I. d. E. S., 2013. Pengaruh Ukuran Butir dan Struktur Kristal terhadap Sifat
Kemagnetan pada Nanopartikel Magnetit (Fe3O4). Prosiding Pertemuan Ilmiah XXVII HFI Jateng &
DIY, Solo, p. 24.

Suryani Taib, d. E. S., 2015. Sintesis Nanopartikel Magnetite (Fe3O4) dengan Template silika (SiO2)
dan Karakterisasi Sifat Kemagnetannya. Indonesian Journal of Applied Physics, 5(1), p. 24.

Ardhiana, dkk. 2014. Spektrofotometri Infra Merah. Laporan Spektrofotometri Infra Merah. FMIPA:
UNP