Feasibility Study of Cockle Shell Powder as a Partial Cement Replacement in Mortar

doi:10.21203/rs.3.rs-5292462/v1

The high demand for mortar in construction necessitates a significant amount of cement. Malaysia has eight cement manufacturers with an estimated production capacity of 40.2 million tonnes. However, natural depletion may occur during the mortar manufacturing process. Additionally, the disposal of seashell waste can negatively impact the environment and contribute to pollution, affecting human quality of life. This study aims to evaluate the feasibility of using marine waste, specifically cockle shell powder (CSP), as a partial replacement for cement in mortar mixtures. The properties of mortar containing varying percentages of CSP (3%, 6%, 9%, and 12%) as a partial cement replacement were investigated. The effects of CSP on workability, compressive strength, and water absorption were analyzed. The findings indicate that the optimum CSP replacement level is 6%, as its properties closely match those of the control mortar, making it an excellent candidate for substitution. However, the experimental results also show that incorporating CSP as a partial cement replacement reduces the workability and strength of the mortar specimens. Furthermore, an increase in CSP percentage corresponds with higher water absorption.

Cockle shell

mortar

cement replacement

workability

compressive strength

water absorption

Cement mortar is composed of cement, sand, water, and admixtures. According to the Brick Industry Association (2020), mortar acts as the bonding agent that integrates bricks into a masonry assembly. It must be strong, durable, and capable of holding the masonry together while providing a water-resistant barrier. Additionally, mortar accommodates the dimensional variations and physical properties of bricks during construction. However, the production of mortar poses significant global challenges. Cement manufacturing, which produces mortar and concrete, consumes considerable energy and generates large quantities of greenhouse gases, with an estimated 1 ton of carbon dioxide (CO₂) emitted per ton of cement produced. This process also contributes to the depletion of natural resources and results in specific waste residues that must be managed (Mohamed & Djamila, 2018).

According to Gillot & Coutelas (2018), mortars are composite materials created by adding water to a mixture of two main components: a binder and a filler. The binder provides consistency and adhesiveness to the mortar, forming a continuous matrix essential for the setting process. While binders alone can be used, fillers, which add bulk, strength, and stiffness, are typically necessary. These fillers usually consist of finely divided minerals or aggregates. Additional components, or additives, are sometimes incorporated to enhance performance or achieve special properties. Water makes the mixture plastic and workable long enough for it to be properly placed and shaped. Once set, the mixture hardens into a solid and relatively permanent material.

Cement content significantly affects the properties of cement mortar. According to Caleb LeBow (2018), cement content plays a crucial role in the mixture, influencing both its fresh and hardened properties. An increase in cement content generally leads to an increase in compressive strength. However, the amount and fineness of cement also impact workability. If a mixture has too much cement relative to its water content, it may be difficult to place. Conversely, if there is too much water, the mixture may segregate, making it challenging to use as intended.

Cockles, specifically the species Anadara granosa, are sea mollusks widely consumed in Southeast Asia. The shells, a by-product of this consumption, represent a significant waste product (Hemabarathy Bharatham, 2014). In Malaysia, cockle shells are abundant due to the seafood industry, yet they remain largely unexploited outside small-scale craft production. The composition of cockle shells includes calcium (Ca), carbon (C), magnesium (Mg), and silica (Si), which are similar to the components found in sand, gravel, and cement (Aniza Mijan, 2011).

To obtain the cementitious benefits of calcium oxide (CaO) for cement hydration, cockle shells are washed, ground, milled, and calcined. Lertwattanaruk (2012) describes a process involving cleaning, grinding, and oven-drying the shells at 110°C. Typical raw seashells contain 95–97% calcium carbonate (CaCO₃) along with small quantities of minerals and organic materials (Olivia, 2017). By burning shells at temperatures above 550°C, CaCO₃ transforms into CaO and carbon. The percentage of CaO in burnt shells ranges from 52–57%, depending on the type and CaCO₃ content. Seashells primarily consist of calcite and aragonite crystals, which have higher strength and density than limestone powder (Hazurina Othman, 2013). Additionally, the particle size of seashells (36–75 µm) is similar to that of Portland cement (Lertwattanaruk, 2012), making cockle shells suitable for use as a cement replacement in mortar mixtures.

Several studies have explored the use of seashells as a partial cement replacement in mortar. D. Binag (2016) investigated the use of oyster, mussel, and mollusk shells in cement mortar, while Lertwattanaruk (2012) examined the use of clam, oyster, mussel, and cockle shells. Research findings indicate that a 5% replacement is the optimum percentage for cement. Both studies reported that the compressive strength of mortar cured for 7 and 28 days was lower than that of control samples, but the results were still acceptable for use in the construction industry.

Absorption testing, such as the BS 1881 − 122: 2011 method for determining water absorption, measures the water-tightness of cement mortar (Kryton, 2014). The use of cockle shells as a cement replacement influences the water absorption properties of the mixture. Abdelouahed (2019) found that increasing the percentage of cockle shells in cement led to higher water absorption due to the increased porosity of specimens. However, at a 20% replacement ratio, water absorption decreased due to reduced capillary voids, resulting from the higher compactness of cockle shell mortar. In cockle shell mortar, capillary voids are critical as they facilitate the development of new products during cement hydration.

This study investigates the properties of cockle shells collected from seafood restaurants in Kuantan, Malaysia. The shells were processed into cockle shell powder (CSP) through washing, grinding, and sieving to 75 µm. The chemical composition and particle size distribution of CSP were analyzed, and the study aims to explore its potential as a partial cement replacement in mortar. The findings may provide solutions for managing cockle shell waste and reducing the reliance on natural resources, ultimately minimizing environmental disruption. The use of CSP in mortar could also lower construction costs compared to using Ordinary Portland Cement.

Materials. In this research, ‘Orang Kuat’ Ordinary Portland Cement of grade 52.5 N, as specified by MS EN 197-1:2014, is used along with fine aggregates of 2.36 mm. Potable water, compliant with BS EN 1008:2002, is sourced from the concrete laboratory of the Faculty of Civil Engineering Technology. Meanwhile, cockle shells are collected from seafood restaurants in Kuantan.

Cockle Shell Powder. The cockle shells must be cleaned and dried. They are then placed in a drying oven at a temperature of 110 ± 5°C for 24 hours. Next, the cockle shells are coarsely ground using a grinding machine until they pass through a No. 4 sieve (4.47 mm). The shells are further ground in a Los Angeles Abrasion machine equipped with a ball mill grinder, rotating with steel balls for 1 to 2 hours, to pulverize the shells until the particles are smaller than a No. 200 sieve (0.075 mm). Figure 1 shows the cockle shell powder.

Mix Design, Specimen Preparation and Testing

Mix Design. A trial method was used to design the mortar with the aim of achieving a target strength of 20 MPa and a plastic consistency. The mix proportions used in the mortar are 3%, 6%, 9%, and 12% of cockle shell powder (CSP). The adopted cement-to-sand ratio is 1:3, and the water-to-cement ratio is 0.7. Table 1 shows the mix proportions of mortar with different percentages of CSP

Table 1

Mix Proportion of Mortar
Mix	CSP (%)	CSP (kg/m³)	Cement (kg/m³)	Water (kg/m³)	Sand (kg/m³)
Mortar	0	0	0.820	0.57	2.72
3 CSP	3	0.015	0.795	0.57	2.72
6 CSP	6	0.050	0.770	0.57	2.72
9 CSP	9	0.075	0.745	0.57	2.72
12 CSP	12	0.100	0.720	0.57	2.72

Specimen Preparation. A total of 60 cubes, each measuring 50 mm x 50 mm x 50 mm, were prepared for the experiment. Three cubes are required to obtain an average reading for each test. The mortar was mixed using a mixer machine. After mixing, the mortar was cast into molds, and the mixture was compacted using a vibrating table to remove any entrapped air and achieve maximum compaction. Each layer was vibrated for approximately 20 seconds. For each percentage of cement replacement, three sample cubes were prepared. The samples were demolded 24 hours after casting and then cured in a water tank for 7 and 28 days at 100% relative humidity and room temperature of 27 ± 2ºC until testing. Figure 2 shows the specimen preparation of the mortar samples.

Flow Table Test. The flow table test was performed to determine the flow of the mortar mixtures according to the ASTM C1437-20, as shown in Fig. 3. The flow spread percentage (%) was calculated by using Eq. 1.

\(\:Flow\%=\frac{(\text{S}\text{p}\text{r}\text{e}\text{a}\text{d}\:\text{d}\text{i}\text{a}\text{m}\text{e}\text{t}\text{e}\text{r}\:\text{i}\text{n}\:\text{c}\text{m}-25)}{25}x\:100\)

(1)

Compression Strength Test. The testing was carried out after the specimens were cured in the tank for 7 and 28 days, following ASTM C109/C109M-20. The specimens before and after the compressive strength test are shown in Fig. 4. The compressive strength ( was calculated by using Eq. 2.

\(\:\sigma\:=\frac{P}{A}\)

(2)

Where,

\(\:\sigma\:\)	Compressive strength of mortar specimen (N/mm²)
P	Maximum load applied (N)
A	Cross-sectional area of mortar specimen (mm²)

Figure 4. Compression Strength Test

Water Absorption Test. Water absorption testing was performed on mortar cube specimens in accordance with the procedure described in BS 1881 − 122. The oven dried and weight specimen are shown in Fig. 5. The water absorption (%) was calculated by using Eq. 3.

\(\:Water\:absoption\:\left(\%\right)=\frac{\text{W}\text{s}-\text{W}\text{d}}{\text{W}\text{d}}\:x\:100\)

(3)

Where,

Ws	Saturated weight of the mortar specimen (kg)
Wd	Dry weight of the mortar specimen (kg)

Morphology Analysis. The microstructural characteristics of CSP mortar were analyzed using Scanning Electron Microscopy (SEM). X-Ray Diffraction (XRD) was also performed to differentiate the amorphous and crystalline components of the samples at room temperature. All tests were conducted at the Centre of Excellence for Advanced Research in Fluid Flow (CARiFF), Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA).

Chemical Composition of CSP. The X-ray fluorescence (XRF) analysis reveals the chemical composition of cockle shell powder (CSP). As shown in Table 2., the predominant oxide in CSP is calcium oxide (CaO), comprising 46.55%, followed by silicon oxide (SiO₂). Other oxides present in CSP include sodium oxide (Na₂O), iron(III) oxide (Fe₂O₃), sulfur trioxide (SO₃), alumina oxide (Al₂O₃), magnesium oxide (MgO), potassium oxide (K₂O), and titanium dioxide (TiO₂), with concentrations of 0.333%, 0.285%, 0.0948%, 0.0771%, 0.0277%, and 0.0232%, respectively. According to Olivia (2017), the calcium oxide (CaO) found in seashells significantly enhances the physical and mechanical properties of the specimens. The amount of CaO is crucial for increasing the density and strength of the specimens. Furthermore, Nasution (2016) notes that the impact strength of the composite improves with higher compositions of cockle shell powder. Notably, cockle shells contain about 99.00% calcium oxide (CaO) (Hazurina Othman, 2013). However, the presence of CaO can also be interpreted as an indication of calcium carbonate (CaCO₃), which is converted to CaO during the thermal decomposition process (Sainudin, 2020).

Table 2

Mix Chemical Composition of CSP
Chemical composition (%)	CSP
Calcium Oxide (Cao)	46.55
Silicon Oxide (SiO₂)	0.819
Sodium Oxide (Na₂O)	0.333
Iron III Oxide (Fe₂O₃)	0.285
Sulfur Trioxide (SO₃)	0.0948
Alumina Oxide (Al₂O₃)	0.0771
Magnesium Oxide (MgO)	0.0277
Potassium Oxide (K₂O)	0.0232
Titanium Dioxide (TiO₂)	-
LOI	-

Particle Size Distribution of CSP. Figure 6 illustrates the particle size distribution of cockle shell powder (CSP). The minimum size distribution of the powder passes through 75 µm. Observations indicate that the sieve size of 0.6 mm contains the highest weight accumulation of cockle shell powder. As the particle size of the ground cockle shell powder decreases, the decomposition rate of the cockle shell increases (M. Mohamed & Yousuf, 2012). Nasution (2016) notes that smaller particle sizes can enhance the composite interface area, thereby increasing impact strength. However, water absorption rises for all particle sizes of cockle shell powder due to the high hygroscopic nature of CSP, which is primarily composed of magnesium oxide (MgO) and calcium oxide (CaO).

Effect of CSP on the Workability. Fresh mortar with varying percentages of cockle shell powder (CSP) as a partial cement replacement was tested using the flow table test to determine workability. The results of the flow table test for the fresh mortar specimens are presented in Fig. 7. The consistency of the control mortar was higher than that of the mortar containing different percentages of CSP. The control mortar had a value of 114%, meeting the standard for mortar. However, when comparing the mortar containing different percentages of CSP, the 6% CSP mixture also achieved a consistency value of 114%, similar to the control. The lowest consistency values were recorded for the 9% and 12% CSP mixtures, with values of 113% and 112%, respectively.

The presence of CSP significantly affects the workability of the mortar, as the flow values decrease when CSP is added to the mixture. This decrease is due to the absorption properties of CSP, which reduce the workability of the mortar mix. According to Hazurina Othman (2013), when cockle shell powder is used, it reduces the water demand, leading to higher workability. However, as the percentage of CSP increases, more water is required. The high calcium oxide concentration in CSP accelerates the cement hydration reaction rate when incorporated into the mixture (Olivia, 2017).

Effect of CSP on the Compressive Strength. Figure 8 shows the compressive strength of the control mortar is higher than that of the mortar containing different percentages of cockle shell powder (CSP). The compressive strength of the control mortar at 7 days was 18.59 MPa. In comparison, the 6% CSP specimen achieved a strength of 18.14 MPa, which is nearly similar to that of the control sample. The lowest compressive strength values for 7 days among the CSP specimens were 14.83 MPa for 3%, 14.64 MPa for 9%, and 14.67 MPa for 12% CSP.

At 28 days, the compressive strength of the control sample was recorded at 23.68 MPa, while the 6% CSP mixture exhibited a strength nearly equivalent to the control sample. The lowest compressive strength values at 28 days for the CSP specimens were 20.55 MPa for 3%, 19.21 MPa for 9%, and 20.81 MPa for 12% CSP. The strength of the mortar increases with longer curing durations. Calcium silicate hydrate (C-S-H), a product of cement hydration, is formed when water reacts with the minerals alite and belite (Silva, 2020). The high CaO content in cockle shell powder can slow down hydration, reducing strength during the early stages of curing. However, the increase in strength becomes more pronounced with extended curing periods (Hazurina Othman, 2013).

According to Lertwattanaruk (2012), increasing the curing time positively affects compressive strength, although the strength remains lower than that of the control sample. Etuk (2012) found that the compressive strength of specimens decreased as the amount of partial replacement increased in the mortar mix. As the percentage of CSP replacement increases, the strength of the mortar specimens tends to decline because cockle shell powder contains less reactive material compared to Portland cement (Abdelouahed, 2019). Based on the testing, the optimum percentage of CSP as a partial cement replacement is 6%, as its compressive strength is nearly equivalent to that of the control sample.

Effect of CSP on the Water Absorption. Figure 9 shows the water absorption of the control mortar is lower than that of the mortar containing different percentages of cockle shell powder (CSP). The water absorption value for the control mortar at 7 days was 11.42%. In comparison, the specimens with 6% and 12% CSP recorded values of 11.53%, which is nearly similar to that of the control sample. The lowest water absorption values for 7 days among the CSP specimens were 10.64% for 3% CSP and 10.14% for 9% CSP.

At 28 days, the water absorption value for the control mortar sample was 9.12%. The 6% CSP replacement exhibited a water absorption of 9.75%, which is close to that of the control sample. In contrast, the 3%, 9%, and 12% CSP specimens recorded higher water absorption values of 11.17%, 11.79%, and 10.09%, respectively. The water absorption at 28 days increased proportionally from the 7-day results for the 3% and 9% CSP replacements, which can be attributed to the higher porosity of the specimens containing cockle shell.

According to Zhang (2019), the porous nature of materials and their permeability significantly influence the rate of absorption and liquid transfer. Therefore, materials with high permeability exhibit a higher absorption rate. For the 6% and 12% CSP replacements, the water absorption value decreased at 28 days due to the increased compactness of the cockle seashell mortar, resulting in a reduced number of capillary voids. Capillary voids are particularly significant in cockle shell mortar, facilitating the formation of new products during the hydration of cement (Abdelouahed, 2019). Overall, the specimen containing 6% CSP exhibited the lowest water absorption, confirming it as the optimum percentage for partial cement replacement.

Microstructural Analysis of Mortar. Scanning Electron Microscopy (SEM) was conducted to analyze the microstructural characteristics of the cockle shell powder (CSP) mortar. Figure 10 displays the morphology of the CSP mortar at magnifications of 5000x and 10000x. From Fig. 10, it can be observed that the CSP mortar exhibits an angular and irregular texture due to the varying particle size distribution resulting from the grinding process. Additionally, it reveals a calcite crystal pattern and structure. According to Hariharan (2014), a solid-state displacement reaction begins during the mechanical milling of the reaction powder mix, leading to irregular particle distribution and form.

Meanwhile, Fig. 11 presents the Energy Dispersive X-ray (EDX) analysis of the CSP mortar. The primary elements in the CSP mortar are composed of Oxygen (59.45%), Carbon (21.65%), Calcium (21.65%), and Silicon (0.98%), with oxygen being the most abundant element. The presence of calcium indicates the incorporation of CSP within the mortar. According to Islam (2011), there are three distinct types of calcium: calcite, aragonite, and vaterite. Ca(OH)₂ can carbonate without an organic substrate, resulting in the formation of calcite crystals. Cockle shells serve as a naturally clean source of calcium carbonate polymorphs, primarily aragonite. However, high temperatures convert the aragonite polymorph to calcite, which is thermodynamically the most stable form (Hariharan, 2014).

XRD Analysis of Mortar. X-Ray Diffraction (XRD) analysis was conducted to determine the crystallization of the cockle shell powder (CSP) mortar. Figure 12 presents the XRD pattern of the CSP mortar. The highest intensity peak, located at 85°, corresponds to Calcium Carbonate (CaCO₃), indicating that CaCO₃ is the main composition in the CSP mortar. The secondary peak at this intensity represents Silicon Oxide, which signifies the crystalline phase present. The CaCO₃ powder derived from cockle shells exhibited well-defined crystallinity, as evidenced by the strong and sharp peaks. According to Hariharan (2014), the calcite phase of CaCO₃ nano powder produced from cockle shells is more stable than the aragonite phase, which is less stable. The quality of calcium carbonate powders produced at the nanoscale may exceed that of powders produced at larger particle sizes, making them suitable for a variety of applications. Lertwattanaruk (2012) notes that seashells, including cockle shells, are potential filler materials due to their high CaCO₃ content, similar to limestone.

Figure 12. XRD Analysis of Mortar

In conclusion, increasing the percentage of cockle shell powder in the mortar mix reduced its workability. Data obtained from the experimental work indicated that higher percentages of cockle shell powder replacement led to a decrease in the strength of the specimens. The experiment successfully determined the water absorption characteristics of the mortar with cockle shell powder as a partial cement replacement. Specifically, water absorption increased with higher percentages of cockle shell powder. The high porosity of the specimens with cockle shell powder contributed to the increased water absorption as the ratio of CSP in the mortar was elevated.

The optimal replacement percentage of cockle shell powder was found to be 6%, as this mixture exhibited compressive strength comparable to the control sample while maintaining acceptable workability. These findings suggest that using cockle shell powder as a partial cement replacement is feasible and can be considered a sustainable alternative in mortar production, potentially addressing both waste disposal issues and reducing reliance on conventional cement.

For further studies, it would be beneficial to investigate the effects of different particle sizes of cockle shell powder on the mechanical properties and workability of mortar. This research could include testing a variety of milling techniques to produce both fine and ultra-fine cockle shell powder.

Author Contribution

Rokiah Othman: Reviews the paper's writing and manages the publication process as the Corresponding Author.Khairunisa Muthusamy: Collects and gathers data, and writes the "Methodology" section of the paper for the first objective.Ramadhansyah Putra Jaya: Analyzes data and writes the "Results and Discussion" section of the paper for the first objective.Youventharan Duraisamy: Collects and gathers data, and writes the "Methodology" section of the paper for the second objective.Mohd Arif Sulaiman: Analyzes data and writes the "Results and Discussion" section of the paper for the second objective.Jeyasaraniya Parsuraman: Collects and gathers data, and writes the paper.Rokiah Othman: Verifies data and reviews the writing of the "Results and Discussion" section of the paper.

Acknowledgement. The author would like to thank Universiti Malaysia Pahang Al-Sultan Abdullah for funding this research through Research Grant RDU230389.

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No competing interests reported.

Feasibility Study of Cockle Shell Powder as a Partial Cement Replacement in Mortar

Status:

Version 1

Abstract

Figures

Introduction

Experimental Programme

Mix Design, Specimen Preparation and Testing

Results and Discussion

Conclusion

Recommendation

Declarations

Author Contribution

References

Additional Declarations

Status:

Version 1