Variation of Polietilena Glikol (PEG) Volume Ratio Addition to the
Extraction and Synthesis of Hematite (Fe2O3) from Iron Ore of
Pemalogan Village using the Precipitation Methods
EDI MIKRIANTO, RAHMAT YUNUS
Department Chemistry Faculty of Mathematics and Natural Sciences,
Lambung Mangkurat University,
A.Yani KM 36 Banjarbaru South Kalimantan,
INDONESIA
Abstract: - The synthesis of hematite iron oxide from iron ore in Pemalongan village was carried out using an
easy and simple method, namely precipitation. The purpose of this study was to determine the extraction
results, crystal structure and crystal size of the compounds synthesized using the precipitation method. Iron ore
processing is carried out by reacting 37% (w/w) HCl by dripping 25% (v/v) NH4OH as a precipitating agent
and adding PEG-200 to control particle size by varying the volume ratio of PEG-200: Iron 1:5 ( mL/g), 2:5
(mL/g), and 3:5 (mL/g). Then calcined at 500°C for 2 hours. The synthesis results were characterized using X-
ray diffraction (XRD) and scanning electron microscopy (SEM). The results of XRD analysis with varying
volume ratios of PEG-200:iron 1:5 (mL/g), 2:5 (mL/g), and 3:5 (mL/g) have formed a hematite iron oxide
phase. The synthesis results with a volume ratio of 1:5 (mL/g) produced the highest purity and had a trigonal
geometric structure, cell parameters a = 5.036340 Å; b = 5.036340 Å; and c = 13.345420 Å; α = β = 90˚; γ =
120˚ and the space group is R3 c. Calculation of crystal size using the Debye Scherrer equation results in
variations in the volume ratio of PEG-200: Iron 1:5 (mL/g), 2:5 (mL/g), and 3:5 (mL/g) is 50.9912 nm;
43.08837 nm; and 45.30663 nm. The SEM characterization results showed that the iron oxide hematite
produced from the synthesis clumped and formed small non-uniform grains.
Key-Words: Iron ore, PEG-200, hematite, extraction, precipitation, synthesis.
Received: September 21, 2022. Revised: January 22, 2023. Accepted: February 24, 2023. Published: March 17, 2023.
1 Introduction
Indonesia is a country with abundant mineral
resources in nature, such as iron ore, [1]. Abundant
iron ore is spread across the islands of Sumatra,
Java, Kalimantan, and some eastern regions of
Indonesia, [2]. Iron ore reserves in South
Kalimantan amount to 7,472,600 tons. Especially in
Bajuin Sub-district, Pemalongan Village, Tanah
Laut Regency has abundant iron ore resources.
However, the iron ore contained still has impurities,
[3] Natural iron ore is generally a compound of iron
with oxygen containing about 73% iron oxides such
as hematite, magnetite (Fe3O4), limonite
(FeO(OH).nH2O), or siderite (Fe2CO3), [2]. Iron ore
is a rock containing iron minerals and a number of
impure minerals such as silica, alumina, magnesia,
and nickel, [4]. One of the most abundant metal
elements on earth is formed around 5% in the earth's
crust, [2]. The benefits of iron ore are as raw
material for making iron and steel, [1], [5]. Hematite
can be used as a dye, [6]. The hematite obtained can
be applied as a ferroelectric material, namely by
using hematite as a mixture for making BiFeO3
ferroelectric materials, [7]. The compound Fe2O3 is
the most stable iron oxide under ambient conditions
so it is commonly used in catalysts, nanocatalysts
[8], photocatalysts to degrade dyes remazol red, [9],
gas sensors, and electrode materials. Fe2O3 is also
commonly used as a basic material for making
permanent magnets, [10].
This research refers to research, [2], namely by
using the precipitation method because the method
has the advantages of being the simplest, easiest,
and cheapest. In his research, iron ore was initially
separated manually (magnetic separation) using a
bar magnet. Furthermore, the separation results were
weighed. Then the iron ore is dissolved in HCl,
while stirring and heating on a hot plate magnetic
stirrer at a certain speed. Precipitation is done by
dripping ammonium hydroxide (NH4OH) into the
solution. After the precipitation occurs, calcination
is then carried out using a furnace. However, the
research to be carried out refers to the research, [11]
before calcination of the precipitate is added first
with polyethylene glycol (PEG). The addition of
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PEG aims to control particle size, so that it can
change the particle size to be small. PEG on the
particles will coat the particles so as to inhibit
growth of the particles. The study succeeded in
obtaining a smaller particle size and causing the
peak formed to be wider. In this study, the volume
ratio of PEG added to the sample mass will be
varied to determine the composition that will form
the optimal result. To get the shape and size of the
particles more uniform, usually, polyethylene glycol
(PEG) is added to the mineral to be synthesized,
[12].
The characterization carried out is by X-ray
fluorescence (XRF) to determine the composition of
the compounds contained in iron ore and
characterization using X-ray Diffraction (XRD) to
determine its crystal structure, [13], [14], then
continued with the Debye Scherrer equation to
determine the particle size, [15]. Characterization of
the crystals obtained was also carried out using the
Rietveld method, [16]. Rietveld method, useful for
matching between theoretical diffraction patterns
and experimental diffraction patterns obtained from
the results of XRD analysis until a match between
the two curves is obtained as a whole. SEM analysis
was carried out to determine the shape of the surface
morphology, [17].
2 Problem Formulation
The problem formulation in this study is as follows:
1. What is the iron content contained in iron ore
from Pemalongan village?
2. What is the structure of hematite (Fe2O3)
extracted and synthesized with the addition of
various volume ratios of PEG-200 using XRD
analysis?
3. What is the crystallinity of hematite (Fe2O3)
extracted and synthesized using the precipitation
method with the addition of variations in the
volume ratio of PEG-200?
4. What is the particle size of hematite (Fe2O3)
extracted and synthesized by adding variation of
PEG-200 volume ratio using Debye Scherrer
equation?
5. What is the morphology of hematite (Fe2O3)
extracted and synthesized using precipitation
method with the addition of PEG-200 volume
ratio variation using SEM analysis?
3 Problem Solution
3.1 Characterization of Iron Ore using XRF
(X-Ray Fluorescence)
Iron ore samples were previously crushed using a
crusher and crushed into fine particles using a tor
mill. Then, iron ore samples were manually
separated (magnetic separation) using a bar magnet,
[2]. Furthermore, the iron ore sample was sieved
using a 200 mesh sieve to get a smaller particle size.
The separation results were weighed as much as 5
grams for XRF (X-Ray Fluorescence) analysis.
Iron ore samples to be extracted were
previously characterized to determine the metal
composition and mineral content contained in iron
ore. The results of XRF analysis are in the form of
qualitative analysis that identifies the types of
elements detected in iron ore, while quantitative
analysis is to identify the number of elements
contained in iron ore which is shown in the element
content in percent (%). The result data was obtained
in the form of graphs and tables detected by X-rays.
The data provides information on the comparison of
metal composition in iron ore before and after the
extraction process.
Iron ore that has been analyzed is then extracted
using the precipitation method. This method is a
chemical separation process, [2]. Iron ore was
previously separated first manually (magnetic
separation) using an oval-shaped magnet. The
purpose of separation is to separate magnetic
minerals from non-magnetic ones. The results of
iron ore separation were then dissolved in 37% HCl
(equations 1), while stirring manually with a glass
stirrer and heated at 90ºC for 60 minutes on a hot
plate, [11]. The following reaction:
Fe2O3 + 6 HCl → 2 FeCl3 + 3 H2O (1)
The addition of 37% HCl to the iron ore aims to
dissolve the entire iron ore. Precipitation is done by
dripping little by little 25% ammonium hydroxide
(NH4OH) into the solution until a precipitate form
(equations 2), with the following reaction:
FeCl3 + 3 NH4OH → Fe(OH)3↓ + 3 NH4Cl (2)
The Fe(OH)3 precipitate formed was filtered
using Whatman No. 42 filter paper. Filtering was
carried out for 6 days to separate the filtrate from the
precipitate. After the filtrate and precipitate were
separated, the precipitate was then washed using
aquademineral. Aqua demineral can not interfere
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with the purity of the synthesis product, because it
does not contain other minerals, which can add
impurities to the synthesis product. The precipitate
was then dried for 16 days. The dried precipitate
was weighed and divided into 3 parts into alumina
crucible, then PEG was added to each sample with
variations in the volume ratio of PEG:Iron 1:5
(mL/g), 2:5 (mL/g), and 3:5 (mL/g). The variation
aims to determine the optimal volume of PEG-200
to produce hematite metal oxide with a smaller
particle size. The addition of PEG-200 to the
particles serves to wrap the particles so that it can
inhibit particle growth, [11]. Furthermore, it is
stirred using a magnetic stirrer for 15 minutes, until
perfect and homogeneous mixing occurs. The
sample that has been obtained is then calcined at 500
◦C for 2 hours using a furnace which aims to
produce a synthesis that has a pure crystal structure
(equations 3). The reaction:
2 Fe(OH)3 → Fe2O3 + 3 H2O↑ (3)
Tabel 1. XRF Characterization Results of Iron Ore
No
Metal
type
Percentage
(%) Before
Extraction
1.
2.
3.
4.
5.
6.
7.
8.
9
Fe
Si
Ca
Cr
Cr
Mn
La
P
Br
97,56 %
0,88 %
0,33 %
0,094 %
0,21 %
0,1 %
0,2%
0,13%
0,53%
The Fe(OH)3 powder obtained was then re-
analyzed using XRF. XRF data on iron ore before
and after the extraction process is shown in Table 1.
Based on the characterization results of XRF (X-Ray
Fluorescence) that have been carried out before
extraction, that Pemalongan iron ore contains
several types of metals such as Si, P, Ca, Cr, Mn,
Cu, Br, La, and the main metal element Fe by
97.56%. Then after extraction, there was a decrease
in other metal elements, even in metal types such as
P, Cu, and Br could be removed and the extraction
process succeeded in increasing the percentage of
the main metal Fe to 97.69%. This is due to the loss
of several other metal elements, causing the
percentage of Fe metal to increase. The samples
obtained from the extraction process were then
synthesized to form hematite metal oxide
compounds. The formed hematite metal oxide was
analyzed for its crystal structure using XRD and
surface morphology analysis of hematite metal
oxide by SEM.
3.2 XRD Characterization Results of
Hematite Iron Oxide Variation of
PEG:Iron Volume ratio 1:5
The results of hematite iron oxide synthesis with the
addition of PEG:Iron volume ratio variation of 1:5
(mL/g) show the presence of hematite iron oxide
phase which can be seen in Figure 1. The 2θ value
shows the angle between the incident ray and the
reflected ray, while the one that shows the number
of X-rays diffracted by the crystal lattice is called
the intensity value. The higher the intensity value
indicates that more crystals are formed and have
good crystal order in the sample. The diffractogram
of the hematite iron oxide synthesis results in a
variation of the PEG:Iron volume ratio of 1:5, which
can be seen in Figure 1. The peaks that appear are
then matched with standard X-ray diffraction data
from JCPDS. The following is a comparison of the
synthesis results with JCPDS data in Figure 2.
Fig.1: Diffractogram of the synthesis results with
variation of PEG:Iron volume ratio 1:5 (ml/g)
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Fig. 2: Comparison of hematite iron oxide synthesis
results of variation of PEG:Iron volume ratio of 1:5
(mL/g) with JCPDS
The results of hematite iron oxide synthesis
variation of PEG:iron volume ratio of 1:5 (mL/g) are
shown on the red vertical line, while the black
vertical line shows the standard hematite iron oxide
synthesis results from JCPDS X-ray diffraction. The
presence of oxide phase peak of hematite iron oxide
synthesis matches the diffraction peak of hematite
iron oxide synthesis with JCPDS data 0.435/13/24
Card # 33-0664.
Based on the results of hematite iron oxide
characterization, the highest intensity was obtained
in the variation of the volume ratio of PEG: Iron,
which was 117.5 with a 2θ angle value of 35.5842°.
The high intensity indicates that the crystal has good
crystal order. In addition, the hematite iron synthesis
with variation of PEG:Iron volume ratio of 1:5
(mL/g) has a higher purity than the hematite iron
oxide with variation of PEG:Iron volume ratio of 2:5
(mL/g). This is indicated by fewer impurity peaks
appearing on the diffractogram pattern. The other
identified impurity phase is Fe3O4. However, based
on the diffractogram, the Fe3O4 impurity has a low
intensity value, so it is not too significant.
3.3 XRD Characterization Results of
Hematite Iron Oxide Variation of
PEG:Iron Volume Ratio 2:5 (mL/g)
The results of hematite iron oxide synthesis with the
addition of variations in the volume ratio of
PEG:Iron 2:5 (mL/g) in Figure 3 show the presence
of hematite iron oxide phase. The peaks that appear
are then matched with X-ray diffraction standards
from JCPDS. The diffractogram of hematite iron
oxide synthesis results with variation of PEG:Iron
volume ratio 2:5 (mL/g), shown in Figure 3.
Based on Figure 3, it can be seen that the
intensity of the resulting peak of hematite iron oxide
is quite low, namely 106.9 with a 2θ angle value of
35.5830, meaning that the hematite iron oxide
product formed is small. This can be caused by
many impurities characterized by the presence of
other peaks that appear on the diffractogram, such as
Fe3O4, SiO2, and CaO. Some of the impurities that
appear may come from extracted impurities that
have not been removed, so the presence of these
impurities can interfere with the process of forming
the target compound. A comparison of the synthesis
results with JCPDS data can be seen in Figure 4.
Fig. 3: Diffractogram of the synthesis results with
the addition of variations in the volume ratio of
PEG:Iron 2:5 (mL/g)
Fig. 4: Comparison of hematite iron oxide synthesis
results of variation of PEG:Iron volume ratio 2:5
(mL/g) with JCPDS
The presence of the hematite iron oxide phase peak
in Figure 4 is similar to the hematite iron oxide
phase peak with JCPDS standard data 0.337/10/24
Card # 33-0664.
3.4 XRD Characterization Results of
Hematite Iron Oxide Variation of
PEG:Iron Volume Ratio 3:5 (mL/g)
The synthesis results on the hematite iron oxide
variation of PEG:Iron volume ratio of 3:5 (mL/g)
has shown the presence of hematite iron oxide phase
as shown in Figure 5.
Based on Figure 5, it can be seen that the
intensity of the hematite iron oxide peak produced is
quite high, namely 114.3 with a 2θ angle value of
35.5932, meaning that the hematite iron oxide
product formed is quite a lot. However, the
synthesized oxide still contains other impurities such
as Fe3O4. However, the impurity peaks that appear
on the diffractogram pattern are fewer. This is
because Fe3O4 from the extraction results still
cannot be removed. Furthermore, the peaks obtained
from the X-ray diffraction data were matched with
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standard X-ray diffraction data from JCPDS. A
comparison of synthesis results with JCPDS data
can be seen in Figure 6.
Fig. 5: Diffractogram of synthesis results with the
addition of variations in the volume ratio of PEG:
Iron 3: 5 (mL/g)
Fig. 6: Comparison of hematite iron oxide synthesis
results of variation of PEG:Iron volume ratio 3:5
(mL/g) with JCPDS
The presence of the hematite iron oxide phase
peak in Figure 11 matches the hematite iron oxide
phase peak with JCPDS data 0.360/12/24 Card # 33-
0664 standard data.
3.5 Comparison of XRD Characterization
Results
The results of hematite iron oxide characterization
by X-ray diffraction with the addition of variations
in the volume ratio of PEG:Iron 1:5 (mL/g), 2:5
(mL/g), and 3:5 (mL/g) show the results of the
formation of hematite iron oxide crystals shown in
Figure 7. The synthesis results in Figure 7 are shown
to have a crystal structure indicated by sharp
diffractogram peaks. From the results of each
synthesis, a comparison of the highest one peak
diffractogram was carried out.
Fig. 7: Comparison of diffractograms of hematite
iron oxide variation of PEG:Iron volume ratio of 1:5
(mL/g), 2:5 (mL/g), and 3:5 (mL/g).
The sharper the peak and the smaller the area,
the higher the crystal quality of the synthesis. Figure
7 shows the highest peak intensity value of the
synthesis at the variation of PEG:iron volume ratio
of 1:5 (mL/g) with an intensity value of 117.5; 2θ =
35.5842o; FWHM of 0.2706, and area of 0.17. The
highest peak of the synthesized 2:5 (mL/g) volume
ratio has an intensity value of 106.9; 2θ = 35.5830o;
FWHM of 0.2713; and an area of 0.17. The highest
peak in the synthesis of 3:5 (mL/g) ratio has an
intensity value of 114.3; 2θ = 35.5932o; FWHM of
0.2833; and an area of 0.18. The highest intensity
indicates that more hematite iron oxide crystals are
formed. states that the highest crystallinity in a
material has a greater number of X-ray reflecting
fields than the same material with a lower level of
crystallinity. To determine the best results, it can be
seen from the FWHM (Full Width at Half
Maximum) value. This FWHM value is related to
the crystallinity value.
Based on Table 2, it can be seen that hematite
iron oxide is synthesized by adding variations in the
volume ratio of PEG: Iron produces hematite iron
oxide with different crystallinity. This can be seen
from the FWHM value and the different areas in
each XRD analysis result.
Table 2. Comparison of hematite iron oxide
synthesis results with variations in PEG:Iron volume
ratios of 1:5 (mL/g), 2:5 (mL/g), and 3:5 (mL/g)
No.
Comparative
factor
Variation of PEG : Iron
Ratio
1 : 5
2 : 5
3 : 5
1.
Peak Position
(2θ)
35,5842
35,5830
35,5932
2.
Intensity
117,5
106,9
114,3
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3.
FWHM
0,2706
0,2713
0,2883
4.
Area
0,17
0,17
0,18
From the results of XRD analysis if the smaller
the FWHM value and area, the higher the
crystallinity value, [18]. In the variation of PEG:Iron
volume ratio 1:5 (mL/g), the hematite iron oxide
formed has the smallest FWHM and area values of
0.2706 and 0.17 compared to the variation of
PEG:Iron volume ratio 2:5 (mL/g), and 3:5 (mL/g).
This indicates that the hematite iron oxide formed
has a good level of crystallinity. Then the highest
intensity value is also in the variation of PEG:Iron
volume ratio of 1:5 (mL/g) which indicates that the
synthesis results in more products produced. Based
on the FWHM value, area, and the highest intensity
value obtained, it can be seen that the hematite iron
oxide synthesis with the best crystallinity is in the
variation of PEG:Iron volume ratio of 1:5 (mL/g).
3.6 Hematite Iron Oxide Crystal Size
The crystallite size with a particular phase can be
done using X-ray diffraction. The determination
refers to the main peaks of the hematite structure of
the diffractogram pattern through the Debye
Scherrer equation approach. To calculate the crystal
size can use the Debye Scherrer equation with the
wavelength, intensity, 2θ, and FWHM values from
the XRD analysis that has been produced. Based on
the calculations obtained, a graph of the relationship
between ln (1/cos θ) as the x-axis and ln β as the y-
axis can be made. The relationship graph of ln
(1/cos θ) with ln β for hematite iron oxide with
PEG:Iron volume ratio variation of 1:5 (mL/g), 2:5
(mL/g), and 3:5 (mL/g) is as follows:
Fig. 8: Particle size graph of hematite iron oxide
variation of PEG:Iron volume ratio of 1:5
(mL/g).
Fig. 9: Particle size graph of hematite iron oxide
variation of PEG:Iron volume ratio of 2:5
(mL/g).
Fig. 10: Particle size graph of hematite iron oxide
variation of PEG:Iron volume ratio of 3:5
(mL/g).
Based on Figure 8, 9 and 10 each sample shows
an R2 value, and a slope value that is not close to 1
and does not have a 45° slope. This indicates that
the 45° slope for a linear line is not achieved. Based
on the data generated, the mismatch of the slope
value and 45° slope is due to the values of β and
1/cos θ not being constant. The β value derived from
FWHM has a different value at each peak, the
FWHM value is influenced by the intensity of each
crystal field. Then the value of 1/cos θ at each main
peak has a different angle. The main thing that
causes this difference is that the electromagnetic
wave hitting the crystal causes diffraction of each
atomic arrangement in the crystal which results in
different X-ray diffraction patterns. R2 and slope
can be close to one with a slope of 45° if the
increase in β value is followed by an increase in
1/cos θ which means that the β value is directly
proportional to 1/cos θ.
This also occurs because the hematite iron oxide
crystals obtained are polycrystalline, which have
more than one crystal orientation with different
scattering fields, causing R2 not to approach one.
Nevertheless, the equation can still be used to
estimate one of the crystal sizes of the
polycrystalline compound. Crystal size data that has
been obtained from the calculation results are as
follows :
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Table 3. Crystal size comparison of iron oxide
synthesis results..
Variation of
PEG : Iron
2θ
FWHM
Crystal
Size (nm)
1:5
35,5842
0,2706
50,99120
2:5
35,5830
0,2713
43,08837
3:5
35,5932
0,2833
45,30663
From Table 3, it can be seen that the addition of
PEG with different volumes in the synthesis process
can produce hematite iron oxide with different
crystal sizes. This shows that the provision of
variations in the volume ratio of PEG affects the
crystal size. The variation of PEG volume ratio
shows that the addition of PEG reaches the optimum
volume at the variation of PEG:Iron volume ratio of
2:5 (mL/g) for an increase in Fe2O3 particles of
43.08837 nm. The decrease in crystal size is related
to the molecular weight of PEG-200. The greater the
molecular weight of PEG, the greater the number of
PEG chains that coat the particle surface. Another
factor that also affects the size of the crystals
produced is the cooling temperature on the rate of
nucleation and the rate of crystal growth. If the
cooling process is fast, the rate of formation of
nuclei is high and the rate of crystal growth will be
faster, resulting in small crystal sizes, whereas in the
slow cooling process, the rate of formation of nuclei
is low, the slow crystal growth process will produce
large size crystals.
3.7 Rietveld Analysis of Hematite Iron
Oxide Variation of PEG: Iron Volume Ratio
1:5 (mL/g)
X-ray diffraction data is then processed by the
Rietveld method using the Rietica program. The
method serves to smooth the calculated diffraction
pattern (model) with the measured diffraction
pattern. From these results, no PEG phase was found
in the sample, meaning that PEG is only useful for
controlling particle size and does not react and only
functions as a template that wraps particles, [19].
Fig. 11: The diffractogram of hematite iron oxide
synthesized by the precipitation method adding a
variation of PEG:Iron volume ratio of 1:5 (mL/g).
From data processing with the Rietveld method,
it produces cell parameters, Miller index, space
group and crystal system (geometry shape) of
hematite iron oxide. Figure 11 shows the Miller
index value showing the hkl value of each dominant
peak at 2θ angles from 10° to 90°. The Miller index
value provides information that shows the position
of atoms in the unit cell and affects the properties
and behavior of the synthesized material.
The diffractogram of the hematite iron oxide
compound synthesized using the precipitation
method that has been processed using the Rietveld
method can be seen in Figure 12. The diffractogram
with black dots is the diffractogram of the
synthesized hematite iron oxide, while the red
diffractogram is the diffractogram of the hematite
iron oxide standard data in the Rietica program,
[14]. The green diffractogram is the diffractogram of
the difference between the data of the synthesized
compound and the standard data of hematite iron
oxide.
Fig. 12: Diffractogram of hematite iron oxide
synthesized using precipitation method with
variation of PEG:Iron volume ratio of 1:5 (mL/g)
processed with Rietica program.
Based on table 4 of data processing using the
Rietica program, it shows that hematite iron oxide
synthesized by the precipitation method with the
addition of variations in the volume ratio of PEG:
Iron 1: 5 (mL / g) has a trigonal geometry with space
group R3 c and cell parameters a = 5.036340 Å; b =
5.036340 Å; and c = 13.345420 Å. Hematite iron
oxide has a trigonal structure. This means that this
crystal structure has 4 axes of symmetry consisting
of 1 main symmetry axis and 3 additional symmetry
axes. The 3 axes (a, b, and d) are the same length
and are located in the horizontal plane while the 1 c
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axis can be shorter or longer as shown in Figure 13.
The trigonal system has an axial ratio, namely a = b
= d ≠ c, meaning that the length of the a axis is equal
to the b axis and equal to the d axis, but not equal to
the c axis and also has crystallographic angles α = β
= 90˚; γ = 120˚. This means that in this system, the
angles α and β are perpendicular to each other and
form an angle of 120˚ to the γ axis.
Table 4. Crystal system, space group, and cell
parameters of hematite iron oxide compounds result.
indexing of Rietica program
Parameters
Iron Oxide
Crystal System
Trigonal
Space Group
R3 c
Parameter Cell Unit (Å)
a : 5,036340
b : 5,036340
c : 13,345420
Angle
𝛼 : 90°
𝛽 : 90°
γ : 120,0000°
Fig. 13: Crystal structure of hematite iron oxide
((Fe2O3))
The results of figure 11 are obtained from the
data in Table 5 which has the following fractional
coordinates.
Table 5. Hematite Iron Oxide Fractional Coordinates
3.8 SEM Characterization of Hematite Iron
Oxide
The results of the synthesis using SEM were carried
out to determine the surface morphology of the solid
sample. The image formed by a very small electron
beam in this analysis is focused on the surface of the
material. The results of SEM analysis with
variations in the volume ratio of PEG obtained have
an influence on crystal morphology. Figure 14
shows that the effect of PEG addition can cause
agglomeration in hematite iron oxide, [20]. The
following morphology of hematite iron oxide
crystals was analyzed using Scanning Electron
Microscope (SEM) with magnification of 10,000
and 20,000 times. Based on Figures 14(a) and 14(c),
the morphology of the synthesized particles with
variations in the volume ratio of PEG:Iron 1:5
(mL/g) and 3:5 (mL/g) shows that particle
agglomeration occurs, causing the particle size to
become large. This is because the pores formed are
smaller. While Figure 14(b) shows that in the
addition of variations in addition to variations in the
volume ratio PEG:Iron 2:5 (mL/g) shows more
particles forming small clumps.
Fig. 14: SEM Characterization Results of hematite
iron oxide (a) 1:5 (mL/g) (b) 2:5 (mL/g) (c) 3:5
(mL/g) with magnification of 10,000 times
WSEAS TRANSACTIONS on ENVIRONMENT and DEVELOPMENT
DOI: 10.37394/232015.2023.19.23
Edi Mikrianto, Rahmat Yunus
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Fig. 15: SEM characterization of hematite iron oxide
synthesis results (a) 1:5 (mL/g) (b) 2:5 (mL/g) (c)
3:5 (mL/g) with a magnification of 20,000 times.
Figures 15(a), 15(b), and 15(c) of hematite iron
oxide synthesis results from SEM characterization
with a magnification of 20,000 times show in more
detail that the hematite iron oxide crystals have
agglomerated. The agglomeration occurs due to the
relatively slow diffusion speed of PEG which causes
the possibility of crystals to agglomerate and
rearrangement occurs which causes smaller pores.
According to [21], the pores in the crystal will
gradually shrink to a smaller pore size, so that the
hematite iron oxide particles (Fe2O3) are
agglomerated. Meanwhile, Figure 15(b) shows that
the crystals do not agglomerate and rather form
small clumps. This is because the more volume of
PEG added, the more PEG is trapped on the surface
of the particles, and during the calcination process
PEG will be decomposed which causes the
formation of pores in the crystal. However, the
presence of pores in hematite iron oxide indicates
that crystals with the addition of PEG at a variation
of the PEG:Iron volume ratio of 2:5 (mL/g) is the
optimum volume, where the resulting particle size is
smaller than 1:5 (mL/g) and 3:5 (mL/g). This is in
accordance with the calculation of Debye Scherrer.
The smallest particle size can be applied as a
catalyst material. According to [22], [23], stated that
different particle sizes and non-uniform morphology
indicate that the addition of PEG has a role in
controlling crystal nucleation, but the results
obtained, PEG has not been seen to have a role in
controlling crystal nucleation.
4 Conclusion
Based on the results of the research and discussion,
the following conclusions can be drawn:
4.1 Conclusion
1. Iron ore from Pemalongan contains iron metal
(Fe) of 97.56%, while the iron metal content after
the extraction process that has been dissolved in
HCl with NH4OH as a precipitating agent is
97.69%.
2. Hematite iron oxide can be synthesized by the
precipitation method, where the structure
obtained by varying the volume ratio of PEG:
Iron 1: 5 (mL / g) has cell parameters, namely, a
= 5.036340 Å; b = 5.036340 Å; and c =
13.345420 Å, and has a space group R3 c with a
trigonal crystal system.
3. Hematite iron oxide synthesized with variation of
PEG:Iron volume ratio 1:5 (mL/g) has the best
crystallinity with FWHM value of 0.2706, and an
area of 0.17.
4. The crystal size of the synthesized hematite iron
oxide calculated by the Debye Scherrer equation
has a crystal size that is in the variation of the
volume ratio of PEG:iron 1:5 (mL/g) of 50.9912
nm, 2:5 (mL/g) of 43.0883 nm, and 3:5 (mL/g) of
45.30663 nm. 5. The morphology of hematite
iron oxide formed tends to agglomerate and has
an inhomogeneous grain distribution.
4.2 Suggestion
Based on the results of the research that has been
carried out, there are several things that can be of
concern for conducting this research, namely further
researchers to vary the calcination temperature to
obtain optimum data resulting from synthesis
products such as high crystallinity
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WSEAS TRANSACTIONS on ENVIRONMENT and DEVELOPMENT
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Edi Mikrianto, Rahmat Yunus
E-ISSN: 2224-3496
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Contribution of Individual Authors to the
Creation of a Scientific Article (Ghostwriting
Policy)
-Edi Mikrianto extracted, synthesized, and analyzed
the structure of hematite iron metal oxide.
-Rahmat Yunus conducted the analysis using XRF,
XRD and SEM instrumentation.
Sources of Funding for Research Presented in a
Scientific Article or Scientific Article Itself
The source of funds comes from the BNBP DIPA
budget of Lambung Mangkurat University.
WSEAS TRANSACTIONS on ENVIRONMENT and DEVELOPMENT
DOI: 10.37394/232015.2023.19.23
Edi Mikrianto, Rahmat Yunus
E-ISSN: 2224-3496
271
Volume 19, 2023
Conflict of Interest
The authors have no conflicts of interest to declare
that are relevant to the content of this article.
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