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ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009

Synthesis and material characterization of calcium carbonate

(CaCO3) from the waste of chicken eggshells

R A Ningrum1, S Humaidi1*, S Sihotang1, D Bonardo1, Estananto2

1
Department of Physics, FMIPA, Universitas Sumatera Utara, Jl. Bioteknologi I
Kampus USU, Medan 20155, Indonesia
2
School of Electrical Engineering and Human Centric Engineering Research Center
Telkom University, Bandung 40257, Indonesia.

*e-mail: syahrul1@usu.ac.id

Abstract. Synthesis and basic characterization of calcium carbonate (CaCO3) material produced
from the extraction of chicken egg shells is proposed. The studied method is applied for the basic
analysis of the mineral CaCO3 in the field of membrane materials. Three basic characteristics of
CaCO3 have been investigated, namely microstructure, crystal structure and vibrational modes.
Microstructure were measured using a scanning electron microscope (SEM), while crystal
structure were measured using an X-ray diffractometer (XRD). Fourier transform infra-red
(FTIR) spectroscopies were used to determine the vibrational modes. Experimental results show
that the morphology of the sample has the characteristics of a microstructure with a mean grain
size of 3 µm, the morphology of the resulting microstructure has a loose spacing between grains
so as to provide an empty space between the sample grains. The crystal structure of CaCO3
formed is trigonal and has a crystal size of 53.306 nm, indicating the formation of nano crystals
in the sample, while the FTIR spectroscopies data show the appearance of the three highest peaks
at wave numbers of 3637 cm-1, 1438 cm-1, and 871 cm-1, which indicates the OH strain functional
groups in Ca(OH)2, CO and calcite groups, respectively. Several studies also reported that the
hydroxyl and carbonation groups at similar wave numbers were 3643 cm -1, 1445 cm-1 and 877
cm-1, and at 712 cm-1, 876 cm-1, and 1425 cm-1 which correspond to C=C, CO, and CS vibrations.

1. Introduction
In the last two decades, the use of functional organic materials in the field of membrane materials has
received great attention from researchers around the world. This is because the cost of making inorganic
membranes is more expensive when compared to organic membranes, besides membranes made from
inorganic materials such as metallic membranes which have a weakness, namely the surface poisoning
effect, then ceramic membranes have disadvantages because they are high sensitivity to temperature
gradients, and materials that often used as membranes such as zeolites also have weaknesses such as
thicker layer requirements to prevent cracks and pinholes and also relatively low gas flux [1]. In fact,
on the other hand, the need for membrane materials is getting higher along with technological
developments in the world.
Pollution is one of the problems faced in modern times, and what is currently the centre of
attention is waste industry. The current rapid growth of the industry is expected to make life easier, it
also brings problems to environmental pollution. Suspended particles are natural pollutants that can fill
the water surface. The presence of these pollutants causes turbidity in the waters. Soil erosion into clay

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ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009

particles originating from the area catchment water is a source of turbidity. The size of colloidal particles
is in the range of a few nanometers to several hundred micrometers, usually colloid ally particles on the
water surface have sizes ranging from 0.001 to 10 microns. Water is a necessity that is needed for
humans, one of which is for toilets for bathing, washing and latrines. The need for clean water for
humans must meet the following requirements: clear, colourless, tasteless, odourless, non-toxic, neutral
pH and free of microorganisms [2]. Along with increasing population and industrial growth, the need
for clean water will continue to increase. If this increase is not balanced with new sources of clean water
supply, it will lead to a clean water crisis. The availability of clean water sourced from surface water is
limited to areas with peat soils. Water on peat soil has the characteristics of dark brown, high organic
matter content, but has a relatively low degree of acidity (pH). Generally, people in areas with peatlands
rely on rainwater for daily consumption, but the availability of rainwater is limited during the dry season.
Due to this condition, the community has no other choice to use the peat water flowing in the
ditches or drainage channels in their neighborhood. In peat water, there are organic substances that can
cause the water to taste sour, for that an alkaline substance is needed to neutralize the acid in peat water.
One of the minerals is egg shell. Egg shells generally have three layers, namely the cuticle, the stratum
layer and membrane layers [3]. Each layer contains separate chemistry. The cuticle layer is the outermost
layer has a thickness of 10 m and a pore channel, and functions protects eggs from moisture and
microorganisms and helps gas exchange into the egg. Egg shell is calcareous layer containing 9-12% of
the total egg weight. The egg shell is composed of approximately 95% calcium carbonate, 1%
magnesium carbonate, 1% calcium phosphate and 4% organic matter especially proteinIt is known that
chicken egg shells contain Calcium Carbonate (CaCO3). This calcium carbonate is alkaline which can
raise the pH of peat water [4]. Almost all of the shells of boiler type chicken eggs contain calcium
carbonate. Based on the calcium carbonate content of the boiler egg shell, if the egg shell is used for
filter media, the treated water can be neutral. Therefore, filter media from chicken egg shells can be used
to improve the quality of peat water for the community so that it can be used for daily activities [5].
It should be noted that research related to CaCO3 sourced from chicken eggshells as a water filter
material is still rarely carried out, this is because CaCO3 is a mineral that can sometimes dissolve in
water. However, due to the hydrophobic nature of egg shells, it can be used as a basis for further research
as a membrane material [4]. Knowledge of the basic material characteristics of CaCO3 synthesized from
chicken eggshells is the core of research in this study, in order to determine and ascertain the functional
side of CaCO3 from chicken eggshells as an organic membrane.

2. Material and Method

2.1. Synthesis of CaCO3 from Chicken Eggshells Waste

All the chemicals used in this study were purchased from Sigma-Aldrich, with an analytical grade
(99.9% purity). Chicken egg shells are collected from several markets in Medan City. In this work, the
mucus from the egg shells was separated by washing it with distilled water. CaCO3 was synthesized
using the simple liquid-solid method. Typically, as-washed eggshells were centrifuged using ethanol
and baked at 80 oC for 50 minutes. Then, the sample was blended until smooth and sieved using a 50
mesh sieve. The as-synthesized powders calcined in the muffle furnace at a temperature of 800 oC for 2
hours at a rate of 1 oC / min.

2.2. Characterizations
The structural properties of CaCO3 sample were studied by using X-ray diffraction (XRD) patterns
recorded using an X-ray diffractometer (Miniflex series Benchtop powder X-ray diffraction Instruments,
Rigaku corporation, Japan) with Cu-Kα radiation (λ = 1.5418 Å). The scanning rate of 5/min was applied
to record the patterns in the range of 7o – 70o. The mean crystallite size of these WO3 samples was
calculated using Debye Scherer’s formula,

2
ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009


D= (1)
 cos

Where k is the shape factor and has a typical value of ∼0.9, λ is the wavelength (Cu Kα = 1.5405 Å), β
is the full width at half maximum of the several peak (in radians), and θ is the Bragg angle of the peak.
For calculation, the several peak was taken for calculation. Then, scanning electron microscope (SEM)
Hitachi SU3500 was used to determine the surface morphologies of CaCO3 sample and the grain size in
each sample was measured through quantitative analysis using the ImageJ application. Vibrational
modes characterization was carried out using the Fourier transform infrared spectroscopy (FTIR) by
taking into account the wave number and intensity. The FTIR spectrum was recorded using room
temperature. The sample of powder is placed into the set holder, then search for the appropriate spectrum
and its effect on the waste water filter media.

3. Results and Discussions

Figure 1. XRD Pattern of CaCO3 powder

Figure 1 is the diffraction pattern of the CaCO3 sample that has been synthesized. CaCO3 powder from
the calcination at a temperature of 800 oC still shows some impurities or compounds, this is indicated
by the presence of several diffraction peaks in other phases besides CaCO3 in the diffraction pattern.
This can occur as a result of a simple synthesis process and not through a long process such as the
hydrothermal method which can optimize the phase purity process [6]. Based on the JCPDS database
No. 05-0586, the crystal structure formed in CaCO3 powder has a trigonal shape and has a diffraction
peak at 2θ: 23.1; 29.4; 31.4; 36.0; 39.4; 43.2; 47.1; 47.5; 48.5; 56.6; 57.4o, where each has a crystal
structure with planes: (012), (104), (006), (110), (113), (202), (024), (018), (116), (211) and (122). In

3
ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009

addition, using Debye Scherrer's formula, the mean crystal size of CaCO3 powder is 53.306 nm. These
results confirm that, a nano-order structure is formed in CaCO3 powder [7].

Figure 2. SEM image of CaCO3 powder with magnification of 5 K

Figure 2 depicts that the resulting morphology of CaCO3 is like a spherical with the grain structure
formed comes from particle stuffing [8]. From the calculation results, the average grain size in the
sample is 3 m, which means that a micron structure is formed in CaCO3. Bonds between grains tend to
agglomerate and are not evenly distributed [9]. This can occur as a result of the synthesis process that
does not allow the aggregation process to occur as is the case with the nanostructure synthesis method
[10].

Table 1. FTIR Spectrum of an Egg Shells with a Calcination Process of 800 °C

Highest Wave Numbers Functional Group of Intensity
Peaks (cm-1) Groups Compounds
1 3637 O-H Alcohol and Phenol 76
2 1438 C=O Ester 57
3 871 C-O Ester and Eter 72

The FTIR used is the Shimadzu brand, where the highest wave number is 3637 cm-1, the O-H functional
group with groups of alcohol and phenol compounds with strong intensity and the third highest wave
number occupies 871 cm-1, the C-O functional group with groups of ester compounds and ether with
strong intensity. This affects the mechanical properties, as an absorbent, increasing pH and decreasing
metal content in wastewater, so that swamp water can be clearer and used for several daily needs [11,12].

4
ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009

Figure 3. Graphic FTIR Spectrum of an Egg Shells with a Calcination Process of 800 °C

Figure 3 shows the FTIR spectrum of an eggshell sample with a calcination process of 800 °C. It can be
seen that the three highest peaks are at wave numbers 3637 cm-1, 1438 cm-1, and 871 cm-1, which show
the O-H strain functional groups in Ca(OH)2, C-O groups and calcite, respectively. Several studies also
reported that the hydroxyl and carbonation groups at similar wave numbers were 3643 cm 1, 1445 cm-1
and 877 cm-1 and at 712 cm-1, 876 cm-1 and 1425 cm-1 which correspond to C=C, CO, and CS vibrations.
The curve confirm the presence of these functional groups at wave numbers 709 cm -1, 871 cm-1, and
1438 cm-1. This indicates that the calcination treatment of CaCO3 leaves more carbon functional groups
in the form of oxygen containing groups [11,13].

4. Conclusion
Mineral CaCO3 has been successfully synthesized using a simple solid-liquid method at 80 oC for 50
min and calcination treatment for 2 hours at 800 oC without any additional template. The microstructure
of CaCO3 granules is formed through a grain degradation process, resulting in an average size of 3 µm.
CaCO3 has a nanocrystal structure with a size of 53.306 nm and has a fairly good purity. The highest
wave number is 3637 cm-1, the OH functional group with groups of alcohol and phenol compounds with
strong intensity and the third highest wave number occupies 871 cm-1, the CO functional group with
groups of ester compounds and ether with strong intensity. This affects the mechanical properties, as an
absorbent, increasing pH and decreasing metal content in wastewater. An improved understanding of
complex interactions and interferences from contaminants to the organic membrane based on CaCO3
under controlled conditions can support the development of compact optimal treatment strategies in the
future.

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ICOSTA 2021 IOP Publishing
Journal of Physics: Conference Series 2193 (2022) 012009 doi:10.1088/1742-6596/2193/1/012009

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