International Journal of Trend in Scientific Research and Development (IJTSRD)

Volume 9 Issue 4, Jul-Aug 2025 Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470

Physicochemical Characterisation and Industrial

Applications of Umuchieze Mined Kaolin Clay
Beneth C. Chukwudi, Briggs M. O. Ogunedo*
Department of Mechanical Engineering, Imo State University, Owerri, Nigeria
*Corresponding Author: Briggs M. O. Ogunedo

ABSTRACT How to cite this paper: Beneth C.

This study comprehensively characterizes the physicochemical Chukwudi | Briggs M. O. Ogunedo
properties of Umuchieze kaolin clay using a suite of analytical "Physicochemical Characterisation and
techniques, including FTIR, SEM/EDS, TGA, and BET analyses. Industrial Applications of Umuchieze
The FTIR results confirm a well-developed kaolinite structure, with Mined Kaolin Clay" Published in
International
distinct silicate framework vibrations in the low-frequency region Journal of Trend in
(640–1163 cm⁻¹) and multiple O–H stretching bands in the high- Scientific Research
frequency region (3620–3691 cm⁻¹), indicative of a highly ordered and Development
silicate matrix with variable hydroxyl environments. SEM/EDS (ijtsrd), ISSN:
analysis reveals a composition dominated by oxygen, silicon, and 2456-6470,
aluminium, consistent with the ideal kaolinite formula, while trace Volume-9 | Issue-4, IJTSRD97369
elements such as carbon, titanium, and iron are present at low levels. August 2025,
TGA demonstrates initial mass loss due to adsorbed water below pp.1004-1015, URL:
100 °C, stability up to 320 °C, and dehydroxylation peaking at www.ijtsrd.com/papers/ijtsrd97369.pdf
480 °C, after which a thermally stable metakaolin phase is formed.
Copyright © 2025 by author (s) and
BET analysis indicates a moderate surface area (~23.76 m²/g) and an International Journal of Trend in
average pore diameter of ~25 nm, confirming a predominantly Scientific Research and Development
mesoporous structure. These findings underscore the material’s Journal. This is an
potential for high-quality paper production, environmental Open Access article
remediation, adsorption processes, and catalytic applications in oil distributed under the
and gas processes. Further studies are recommended to optimize terms of the Creative Commons
surface modification and beneficiation techniques, thereby enhancing Attribution License (CC BY 4.0)
its performance in these advanced industrial applications. (http://creativecommons.org/licenses/by/4.0)

KEYWORDS: Kaolin, Kaolinite, metakaolin, dehydroxylation,

Adsorption, paper production, physicochemical properties.

1. INTRODUCTION
Kaolin clay is a versatile industrial material renowned hexagonal arrangement. As seen in figure 1, each
for its unique physico-chemical properties, which tetrahedron shares three oxygen atoms with adjacent
have led to its widespread use in ceramics, paper, tetrahedra, while the fourth oxygen bonds with
rubber, cosmetics, pharmaceuticals, and aluminium in the octahedral sheet. The O Sheet is
environmental remediation [1–3]. Derived from the composed of Al2O₆ octahedra, where aluminium
weathering of feldspathic rocks, kaolin primarily (Al³⁺) is surrounded by six hydroxyl groups (OH⁻) or
consists of kaolinite an aluminosilicate mineral with oxygen atoms. This sheet forms a gibbsite-like layer
the chemical formula Al₂Si₂O₅(OH)₄ and a that interacts with the tetrahedral silica layer above it.
characteristic two-dimensional layered structure [4]. As depicted in figure 1, the tetrahedral and octahedral
It has a 2:1 (T-O) structure, meaning it is composed sheets are linked together via shared oxygen atoms,
of alternating tetrahedral (T) silica and octahedral (O) forming one structural unit. Multiple units are stacked
alumina sheets. Kaolin consists of stacked layers, together through hydrogen bonding, creating a non-
each made up of two fundamental sheets. The T Sheet swelling structure and platy morphology
made up of SiO₄ tetrahedra linked together in a characteristic of kaolin.

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Fig. 1: Illustration of a kaolin structure.

Kaolin high whiteness, low abrasiveness, and good thermal stability have been instrumental in ensuring product
quality in various industries, while its chemical inertness and high cation exchange capacity further enhance its
applicability in environmental cleanup processes [6,7].
Despite the extensive global utilization of kaolin, the physico-chemical properties of this material can vary
significantly with the geological origin of the deposits, necessitating thorough characterization to optimize its
industrial use [8]. Advanced analytical techniques such as Fourier-transform infrared spectroscopy (FTIR)
[9,10], scanning electron microscopy (SEM) [11], Brunauer–Emmett–Teller (BET) analysis [6], and
thermogravimetric analysis (TGA) [12] are critical for elucidating the mineralogical composition, structural
features, thermal behaviour, and chemical makeup of kaolin clays. Such comprehensive studies not only enhance
the fundamental understanding of kaolin but also facilitate the development of targeted beneficiation and
processing strategies tailored to specific industrial applications.
Nigeria is endowed with abundant kaolin reserves as shown in the mineral resources map in figure 2 [13].

Fig. 2: Mineral resources map of Nigeria showing location of kaolin deposits in Imo state [13].

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Reports exist on the characterisation of some of these Kaolin reserves in places such as Ijero-Ekiti, Ikere-Ekiti,
Isan-Ekiti, Abusoro and Odigbo [14], Auchi [15], Alkaleri [16], Nsu [17], Eha-Ndiagu [18], Lakiri [19], Kaoje
[20], Ifon [21], Avutu Obowo [22], Akoko [23], Umuoke Obowo [24], Kankara [25], Ijero-Ekiti, Ode-Irele, and
Iwo[26], Nsu, Onuiyi Obowo, Nkumeato, Oboro, Kutigi, and Afuze [27], Okpella [28]. These studies present a
significant yet underexploited resource, with many deposits remaining inadequately characterized. One such
deposit is located in Umuchieze in Ihitteafoukwu Ekwerazu Ahiazu Mbaise of Imo state, in the southeastern
region of Nigeria. Although the region is recognized for its rich mineral endowment, detailed investigations into
the properties and potential industrial applications of Umuchieze kaolin is yet to be studied and is not captured in
the mineral resources map of Nigeria as shown in figure 1. Addressing this gap, the present study aims to
provide a detailed physico-chemical characterization of kaolin clay from the Umuchieze deposit. Through the
application of advanced analytical methods, the study seeks to delineate the material’s mineralogical and
structural characteristics, thermal stability, and chemical composition, thereby assessing its suitability for a range
of industrial applications.
The outcomes of this research are anticipated to offer critical insights into the performance of Umuchieze kaolin,
potentially bolstering local industrial processes and reducing reliance on imported raw materials. Furthermore,
the study underscores the broader significance of characterizing indigenous mineral resources in developing
countries, contributing to sustainable economic growth and the advancement of environmentally compatible
technologies in both local and international markets.
2. Materials and Methods
2.1. Sample Collection and Preparation
Kaolin clay samples were collected from various locations within the Umuchieze mining site to ensure
representativeness. The samples were air-dried to remove moisture, ground using a mortar and pestle, and sieved
to achieve a uniform particle size distribution (less than 75 µm).
2.2. Fourier Transform Infrared Spectroscopy (FTIR)
FTIR analysis was performed to identify functional groups, and chemical bonds present in the kaolin clay.
Spectra were recorded in the range of 4000–600 cm⁻¹ using a Nicolet Avatar 360 FTIR spectrometer at a
resolution of 4 cm⁻¹, with 50 scans per measurement in triplicates. Each spectrum was acquired by subtracting
the background from the original spectrum.
2.3. Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS)
The surface morphology and elemental composition of the samples were characterized using a Carl Zeiss
evo10LS-EDAX scanning electron microscope equipped with energy-dispersive spectroscopy (EDS). Prior to
imaging, the samples were sputter-coated with a thin layer of gold to enhance conductivity. SEM micrographs
were acquired at magnifications ranging from 500× to 5000× to elucidate the sample morphology, and
subsequent EDS mapping provided semi-quantitative elemental analysis of the materials.
2.4. Thermogravimetric Analysis (TGA)
Thermal stability and compositional analysis were assessed using thermogravimetric analysis. Approximately 10
mg of the kaolin sample was placed in a platinum crucible and heated from room temperature to 800°C at a rate
of 10°C/min under a nitrogen atmosphere. Weight loss data were recorded to identify phases such as
dehydroxylation and other thermal events.
2.5. Pore structure analysis
The specific surface area, pore size distribution, and total pore volume of the kaolin samples were determined
using BET analysis. Approximately 0.5 g of sample was degassed at 120°C for 12 hours under vacuum before
nitrogen adsorption-desorption measurements were carried out using a micromeritics Tristar 3000 V4.02 surface
area analyser. The specific surface area (SBET) was determined by applying the Brunauer–Emmett–Teller
(BET) method within the relative pressure range of 0.05–0.20 [31]. The total pore volume (Vp) was estimated
from the amount of nitrogen adsorbed at a relative pressure (p/p₀) of 0.99. The pore size distribution and average
pore diameter were derived using the Barrett–Joyner–Halenda (BJH) method [32].
3. Results and Discussion
3.1. FTIR result: The FTIR spectrum of the kaolin clay sample as shown in figure 3 exhibits several well-
defined absorption bands that can be correlated with the vibrational modes of the mineral’s structural
constituents.

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Fig. 3: FTIR spectrum of Umuchieze mined kaolin clay

In the low-frequency region (640–1163 cm⁻¹), the observed bands are primarily associated with the bending and
stretching vibrations of the silicate framework and metal–oxygen bonds:
 640 cm⁻¹: This band is attributed to Al–O bending vibrations, likely arising from distortions within the
octahedral sheet.
 675 cm⁻¹ and 748 cm⁻¹: These absorptions are assigned to Si–O–Al bending vibrations, reflecting the
interactions between the tetrahedral and octahedral layers of kaolinite.
 790 cm⁻¹: This peak is indicative of the symmetric stretching of Si–O–Si bonds within the tetrahedral sheet.
 908 cm⁻¹: Typically, a band in this region corresponds to the in-plane bending vibrations of inner hydroxyl
groups.
 935 cm⁻¹, 997 cm⁻¹, and 1026 cm⁻¹: These bands are associated with the stretching vibrations of Si–O bonds
in the silicate framework, confirming the presence of a well-developed tetrahedral network.
 1114 cm⁻¹ and 1163 cm⁻¹: These peaks further corroborate the presence of Si–O stretching modes. The band
at 1163 cm⁻¹ may also suggest minor contributions from quartz impurities or reflect asymmetrical stretching
vibrations characteristic of kaolinite.
The mid-frequency region includes the 1600 cm⁻¹ band, which is commonly ascribed to the bending vibrations
of adsorbed or structurally bound water molecules, a typical feature in clay minerals.
In the high-frequency region, four distinct bands are observed at 3620 cm⁻¹, 3651 cm⁻¹, 3670 cm⁻¹, and 3691
cm⁻¹. These bands are unambiguously assigned to the O–H stretching vibrations of the inner-surface hydroxyl
groups within the kaolinite structure [29]. The presence of multiple peaks in this region reflects the existence of
hydroxyl groups in different chemical environments, which is attributable to variations in hydrogen bonding and
the local coordination geometry within the layered silicate structure. This also suggests a highly structured
kaolinite mineral [30]. The consistency of the observed peak positions with those reported for typical kaolinite
[10,29–32], confirms the mineral's characteristic structural features, including its silicate framework and distinct
hydroxyl environments. Consequently, the FTIR spectral analysis not only validates the presence of a highly
structured kaolinite material in the sample but also provides insight into the subtle structural variations that may
influence its physico-chemical properties and subsequent industrial performance.
3.2. SEM and EDS result: The combined spectroscopic and microscopic analyses of the kaolin clay sample
reveal a comprehensive picture of its structural and compositional attributes, which are critical for its
industrial performance. The FTIR spectrum confirmed the presence of characteristic vibrational modes
associated with the kaolinite structure specifically, the O–H stretching vibrations (3620–3692 cm⁻¹)
indicative of multiple hydroxyl environments and the silicate framework vibrations (640–1163 cm⁻¹).
These observations were further corroborated by SEM and EDS analyses, which provided a semi-
quantitative elemental composition of the material as follows: Oxygen (59.9%), Silicon (17.3%),
Aluminium (12.7%), Carbon (7.3%), Titanium (1.5%), and Iron (1.4%) as seen in figure 4.

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Fig. 4: SEM and EDS of Umuchieze kaolin clay

The dominance of oxygen, silicon, and aluminium in the EDS spectrum aligns well with the ideal kaolinite
formula, Al₂Si₂O₅(OH)₄, where a robust silicate network is expected. Although the measured weight percentages
of silicon and aluminium are somewhat lower than the theoretical values, this discrepancy is typical of surface-
sensitive techniques like EDS, which may underestimate light element contributions due to limitations in
detector sensitivity and the potential influence of surface roughness or contamination [33]. The detection of
carbon at 7.9% likely originates from surface contamination or residual organic matter, which is commonly
observed in EDS analyses of clay minerals [34]. While this carbonaceous layer can potentially affect optical
properties particularly brightness, which is a critical parameter for paper production its impact can be minimized
through further purification or controlled processing.
Moreover, the trace amounts of titanium (1.5%) and iron (1.4%) suggest minor isomorphic substitutions or the
presence of discrete impurity phases. In paper manufacturing, elevated levels of Fe and Ti can adversely affect
the brightness and colour of the final product; however, their low concentrations in this sample imply that, with
appropriate beneficiation, the clay can meet the stringent quality requirements for high-grade paper coatings.
Conversely, in environmental remediation and catalysis applications, these trace elements might enhance the
clay’s reactivity by providing additional catalytic sites or modifying the surface charge distribution, thereby
potentially improving adsorption efficiency and catalytic turnover. These results, along with FTIR data showing
hydroxyl and silicate bands, suggest the Umuchieze kaolin sample is mainly kaolinite but with potential
impurities.
3.3. TGA result: The TGA curve as shown in figure 5 exhibits an initial mass loss occurring between 32 °C
and 100 °C, which is typically attributed to the removal of physically adsorbed water. This behaviour is
consistent with the expected moisture content in clay minerals and supports the presence of loosely bound
water molecules, as indirectly inferred from the FTIR absorption near 1600 cm⁻¹ often associated with the
bending vibration of water molecules.

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Fig. 5: TGA profile of Umuchieze kaolin clay

Following this initial phase, the sample shows negligible mass loss until the temperature reaches approximately
320 °C. This plateau indicates that the kaolin clay maintains its structural integrity in this temperature range,
implying that no significant chemical transformations or loss of bound water occurs under moderate heating
conditions. This stability is advantageous for industrial processes that require drying or moderate thermal
treatment, such as in paper coating applications [7]. A pronounced mass loss is observed beginning at around
320 °C, which peaks at approximately 480 °C. This temperature range corresponds to the dehydroxylation
process of the kaolinite structure the loss of structural hydroxyl groups (–OH) from the octahedral sheet. The
FTIR data, which exhibited distinct O–H stretching bands in the high-frequency region (3620–3692 cm⁻¹),
confirm the presence of these hydroxyl groups. The dehydroxylation peak at 480 °C is indicative of the
transformation of kaolinite into metakaolin, a process well-documented in the literature Moore & Reynolds [35].
This transformation is critical for applications requiring thermally activated materials, such as catalysts or
adsorbents, where changes in surface chemistry and reactivity can be exploited. After 480 °C, the TGA curve
levels off, showing no further significant mass loss up to 800 °C. This thermal stability beyond the
dehydroxylation stage implies that the resultant metakaolin phase is resistant to further thermal decomposition.
Such stability is crucial for high-temperature industrial applications, including certain catalytic processes and
ceramic formulations.
3.4. BET analysis: The measured BET surface area has a value of ~23.76 m²/g which is considered to be
moderate and aligns well with the expected range for kaolinite clays that have not undergone extensive
activation or delamination [36]. The average pore diameter of approximately 25 nm situates the material
firmly within the mesoporous regime (2–50 nm) [37]. This mesoporosity is crucial for several industrial
applications, as it facilitates the diffusion of reactants and products in catalytic and adsorption processes.
The total pore volume of 0.1497 cm³/g further supports the presence of an interconnected pore network,
which can be particularly beneficial in processes such as environmental remediation, where the adsorption
of contaminants relies on accessible pore channels.

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Fig. 6a: Liquid Nitrogen Physisorption Isotherm

The nitrogen physisorption isotherm of the kaolin sample, as depicted in figure 6a, exhibits characteristics of a
Type V isotherm according to the IUPAC classification [38]. This classification is supported by the observation
of 3 regions viz: Low-pressure Region (P/P₀ < 0.4) were the isotherm shows a slow initial uptake, which is
consistent with weak physisorption interactions. Intermediate pressure region (P/P₀ ~ 0.4 to 0.8) where there is a
steady increase in adsorption, likely due to multilayer adsorption rather than strong monolayer formation.
Finally, high-pressure region (P/P₀ > 0.8) where a significant increase in adsorption occurs, indicative of
capillary condensation in mesopores. The Type V isotherm is typically associated with materials where the
adsorbate-adsorbent interactions are relatively weak, as seen in hydrophobized or poorly hydroxylated surfaces
[14,39], certain modified clays [40], and some silica-based materials [41,42]. Additionally, the isotherm exhibits
a noticeable hysteresis loop, which occurs due to the difference between the adsorption and desorption pathways.
This loop is characterized by a steep desorption branch without a clear plateau at high relative pressures (P/P₀ >
0.8). It is commonly observed in aggregates of plate-like particles forming slit-shaped pores, which is typical of
clays, layered silicates, and certain carbon-based materials [39]. Since kaolin has a layered structure, it is highly
likely that the sample exhibits a Type H3 hysteresis loop, indicating mesoporosity due to slit-shaped voids
between stacked kaolinite layers.

Fig. 6b: BJH desorption pore size distribution plot of the kaolin material
The BJH (Barrett-Joyner-Halenda) desorption pore size distribution plot depicted in figure 6b provides valuable
insights into the pore structure of the kaolin material, particularly regarding mesoporosity and the nature of its
porous network. From figure 6b, the peak pore diameter appears to be around 15–20 nm, indicating that the
kaolin material predominantly contains mesopores (2–50 nm). A gradual decline in dV/dlogD at larger pore
diameters suggests the presence of some larger mesopores and possibly macropores (>50 nm). Furthermore, the
steep initial increase followed by a gradual decline suggests a dominance of slit-shaped mesopores, which aligns

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with the Type V isotherm and H3 hysteresis loop observed in the nitrogen adsorption-desorption isotherm. This
type of pore network suggests limited pore interconnectivity, meaning that adsorption behaviour may be
influenced by restricted diffusion pathways [38]. It is observed also that there is no significant peak at pore
diameters below 2 nm, confirming that the material does not contain a substantial fraction of micropores. This
aligns with the BET surface area result (~23.76 m²/g), which is moderate and indicates the absence of highly
microporous structures.
4. Suitability of Umuchieze kaolin for industrial adsorption sites for larger organic pollutants and dyes.
applications However, its efficiency in gas-phase adsorption may
The comprehensive physicochemical analysis of the require surface modification. The material’s moderate
Umuchieze kaolin clay suggests its suitability for pore volume suggests a balance between adsorption
diverse industrial applications, including high-quality capacity and mechanical stability, which is
paper production, environmental remediation, particularly beneficial in wastewater treatment
adsorption processes, and catalytic systems. The applications. Post-dehydroxylation thermal treatment
structural integrity, surface chemistry, and thermal can enhance surface reactivity, increasing adsorption
stability of the material play critical roles in efficiency through additional active site formation.
determining its industrial relevance.
4.3. Catalysis: The kaolinite structure provides a
4.1. Paper production: The structural framework of stable framework suitable for catalytic
the kaolin, as indicated by FTIR and SEM/EDS applications, particularly after thermal
data, demonstrates sufficient mechanical activation. The presence of hydroxyl groups
stability for use in durable coatings. While the ensures potential active sites for catalysis, while
presence of trace impurities such as carbon, trace levels of iron and titanium may contribute
iron, and titanium may slightly reduce optical to redox reactions. The TGA results confirm
brightness, their low concentrations suggest the transition from kaolinite to metakaolin at
that further refinement via flotation or acid elevated temperatures, leading to the
leaching can enhance the material’s brightness development of an enhanced porous structure
to meet industry standards. that can be further functionalized with catalytic
Thermal analysis confirms that the kaolin maintains species.
structural stability below 320°C, which is beneficial The BET analysis indicates a moderate surface area
for its processing in paper manufacturing. The low with a well-defined mesoporous network, which
abrasiveness of the material ensures minimal wear on supports its potential use as a catalyst support. The
production equipment, a key requirement in the paper Type V isotherm and the corresponding mesoporous
industry. The moderate BET surface area is structure suggest that the material could be employed
advantageous, as excessive surface reactivity could in diffusion-controlled catalytic processes.
interfere with organic binder interactions, potentially Functionalization strategies such as acid activation or
affecting coating smoothness. The mesoporous transition metal doping may be necessary to optimize
structure enhances ink absorption and printability, catalytic efficiency.
making it a promising candidate as a filler or coating
4.4. Ceramics and coatings: The pore size
pigment. However, surface treatment may be required
distribution and structural stability of the kaolin
to improve dispersion and uniformity within
material suggest its suitability for ceramic
papermaking slurries.
applications. The controlled porosity
4.2. Environmental remediation and adsorption: The contributes to mechanical strength and thermal
presence of surface hydroxyl groups, as stability, essential characteristics for high-
confirmed by FTIR, provides reactive sites for performance ceramic components. The
pollutant adsorption. The elemental moderate surface area and stable mesoporous
composition derived from SEM/EDS analysis structure further enhance its applicability in
indicates a stable kaolinite matrix capable of coatings where thermal resistance and
adsorbing heavy metals and organic controlled permeability are required.
contaminants. Additionally, the trace levels of
5. Conclusion
iron and titanium oxides may contribute to
The comprehensive characterization of the
enhanced surface reactivity under optimized
Umuchieze kaolin clay confirms a well-developed
conditions.
kaolinite structure, as evidenced by FTIR analysis
The mesoporous structure, with an average pore that revealed distinct silicate framework vibrations
diameter of 25nm, facilitates the accessibility of (640–1163 cm⁻¹) and diverse O–H stretching bands

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(3620–3691 cm⁻¹), indicative of a highly ordered and Consent to Participate declaration
stable mineral. SEM and EDS analyses corroborated Not applicable
these findings by demonstrating a composition
Clinical trial number
consistent with the ideal kaolinite formula dominated
Not applicable
by oxygen, silicon, and aluminium with trace levels
of carbon, titanium, and iron that, with proper Data availability declaration
beneficiation, are unlikely to hinder industrial The datasets generated during and/or analysed during
performance. Thermogravimetric analysis further the current study are available from the corresponding
established the material’s thermal stability, showing author on reasonable request.
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