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Article

Effect of Olive Waste Ash as a Partial Replacement of Cement on the Volume Stability of Cement Paste

by
Safa Ghazzawi
1,
Hassan Ghanem
1,*,
Jamal Khatib
1,2,
Samer El Zahab
3 and
Adel Elkordi
1,4
1
Faculty of Engineering, Beirut Arab University, 12-5020 Beirut, Lebanon
2
Faculty of Engineering, University of Wolverhampton, Wolverhampton WV1 1LY, UK
3
College of Engineering and Technology, American University of the Middle East, Egaila 54200, Kuwait
4
Faculty of Engineering, Alexandria University, Alexandria 5423021, Egypt
*
Author to whom correspondence should be addressed.
Infrastructures 2024, 9(11), 193; https://doi.org/10.3390/infrastructures9110193
Submission received: 28 August 2024 / Revised: 30 September 2024 / Accepted: 24 October 2024 / Published: 29 October 2024
(This article belongs to the Special Issue Sustainable and Digital Transformation of Road Infrastructures)
Browse Figures
Versions Notes

Abstract

:
Over the last decades, concrete has been excessively prone to cracks resulting from shrinkage. These dimensional changes can be affected by the incorporation of supplementary cementitious materials. This work used olive waste ash (OWA), which could substantially tackle this problem and achieve sustainability goals. For this issue, five cement paste mixes were prepared by replacing cement with OWA at different percentages varying from 0 to 20% by weight with a constant increment of 5%. The water-to-cement ratio was 0.45 for all mixes. Compressive strength and flexural strength were investigated at 7, 28, and 90 days. In addition, three shrinkage tests (drying, autogenous, and chemical) and expansion tests were also conducted for each mix and measured during 90 days of curing. The experimental findings indicated that there was a loss in compressive and flexural strength in the existence of OWA. Among all mixes containing OWA, the samples incorporating 10% OWA exhibited maximum strength values. Furthermore, the chemical and autogenous shrinkage decreased with the incorporation of OWA. However, the drying shrinkage decreased at lower levels of substitutions and increased at higher replacement levels. In addition, there was a growth in expansion rates for up to 10% of OWA content, followed by a decrease at higher levels (beyond 10%). Additionally, correlations between these volumetric stability tests were performed. It was shown that a positive linear correlation existed between chemical shrinkage and autogenous and drying shrinkage; however, there was a negative relationship between chemical shrinkage and expansion.

1. Introduction

Volume stability is an intrinsic engineering property that directly affects the serviceability and long-term durability of various cement-based materials. This has motivated researchers to widely focus their studies on the shrinkage performance of concrete structures, including chemical-, drying-, and autogenous-shrinkage as well as expansion. Thus, concrete can expand or contract excessively in light of changes in the moisture content, temperature, and chemical reactions [1,2,3,4,5,6,7,8,9]. By definition, drying shrinkage is the contraction behavior of the concrete during the hardening period, which is likely to be associated with the internal loss of water by evaporation [1]. It is affected by many parameters such as humidity, the size of the specimen, water-to-cement ratio, and paste volume [1]. Autogenous shrinkage is defined as a reduction in the dimensions (volume or length) of cementitious materials without any transfer of moisture to the surrounding environment [2]. As cement hydration progresses, the matrix enters the stage of self-desiccation independently of external conditions; therefore, this type of shrinkage can also be known as self-desiccation shrinkage [3]. Chemical shrinkage is well-defined as the internal early change in the volume of cement-based materials due to the hydration process [4,5]. The cement composition is the principal influence factor on the development of chemical shrinkage [6]. Three methods are mainly applied to measure the chemical shrinkage rate: dilatometry, pycnometry, and gravimetry [5]. The dimensional change that occurs when the specimen is exposed to excess moisture or water is known as “expansion” [7]. Generally, the moisture content and the change in temperature of the relative humidity have significant effects on the mechanism of the expansion [8,9].
Extensive studies have assessed the effect of supplementary cementitious materials (SCMs) on shrinkage magnitudes, and its trend has changed depending on the quantity of the SCM included. It was displayed that concrete made with clay and limestone fines presents high autogenous shrinkage strains compared to the control concrete [10]. The influence of limestone fines (LF) replacing cement in both mortar and paste on the four types of shrinkage has been examined as well [11,12,13,14]. The outcomes revealed an improvement in chemical shrinkage for 15% of LF for both cement paste and mortar, and, for up to 10% inclusion, an increase in autogenous shrinkage occurred [11,12,13,14]. However, the drying shrinkage increased as LF content increased, and noticeable changes in expansion were observed with replacements surpassing 15% of LF [11,12,13,14]. Moreover, it was stated that fly ash replacing ordinary cement in concrete had a good performance in terms of lowering drying shrinkage [15]. Another experimental work reported that in the presence of nano-silica, the chemical shrinkage gradually rose in the first curing days [16]. The effects of furnace bottom ash (FBA) used as a natural sand substitute on the drying shrinkage of concrete were also investigated: the results indicated that as FBA content increased, the rate of drying shrinkage increased [17]. Additionally, the normal cement was partially replaced by combining fly ash (FA), blast furnace slag (BFS), and metakaolin (MK) to produce green concrete with lower drying shrinkage, reducing structural cracking [18].
Lebanon is famous for its olive tree agricultural sector and the olive oil production process, which produces huge amounts of olive oil residues. One of these wastes is “pomace”, which is burned to obtain OWA. Actually, this local material contains complex organic components that are difficult to decompose when disposed of in landfills, thereby, causing harm to the ecosystem. The literature review presents a lack of using OWA as a cement substitute in cement-based materials for volumetric change investigation for sustainability purposes. Recently, OWA has been gaining increased interest in light of its efficient properties and environmental friendliness, which is characterized by its pozzolanic reaction, filler effect, and low-cost effectiveness [19,20]. In general, pozzolanic materials are natural or industrial resources essentially consisting of silicon (SiO2) and aluminum (Al2O3) oxides [21]. This material, when mixed with water, reacts with the hydrate products to form a calcium–silicate–hydroxide (C-S-H) gel responsible for strength-development and durability purposes. The stronger the pozzolanic action is, the more attractive it is for diverse applications including building construction, soil stabilization, and production of geopolymers. A previous study reported that OWA was beneficial in enhancing the workability of cement paste [19]. Another research carried out on rammed earth blocks showed that OWA possessed cementitious and pozzolanic behavior and improved its mechanical performance [20]. Additionally, olive waste biomass ash could behave as a filler in self-compacting concrete, resulting in a compressive strength similar to that of the reference mix [21].
In addition to the described mechanical functionality of OWA, shrinkage parameters using different levels were previously examined. A prior investigation was made on non-structural recycled concrete with low replacement percentages of natural sand with olive biomass bottom ash (0, 3, and 6%) yielding a higher drying shrinkage value [21]. On the other hand, the paste expansion tended to drop with the addition of OWA at various levels ranging from 3 to 15% [22]. Another assessment aimed to manufacture cement mortar using different treated biomass bottom ash (BBA) [23]. The laboratory results indicated that OWA contributed to the occurrence of high dimensional changes compared to the control mix [23]. In self-consolidating concrete production, this effect could also be explained by the filler effect of the ash, which inhibited water evaporation [24]. On the other hand, in brick manufacturing, the specimens made with 20% olive pomace bottom ash (OPBA) exhibited the highest linear shrinkage [25]. Olive biomass bottom ash (BBA) was used as an economic agent for expansive soil stabilization in the construction of road embankments due to its capacity to reduce the expansion of soils [26]. Furthermore, BBA was used in mortar specimens to examine its effect on mechanical performance using varying factors [27]. These factors included the type and content of cement implemented (515, 485, and 450 g/L) and the percentage of replacement of sand or cement with BBA (0, 10, and 20%). The findings indicated that the increase in BBA content decreased porosity, density and compressive and flexural strengths. Also, the decline in porosity and density was strongly correlated to the high absorption water of this ash [27]. Another study used pomace and olive kernel as alternatives to cement with percentages of 10 and 30% by mass to fabricate mortars with better stiffness [28]. Based on the evaluation tests, adding 10% of these two alternatives approximately maintained the compressive strength of the control mixture (around 50 MPa). Additionally, the influence of particle size was investigated. As a result, after two hours of milling, the residual for ordinary cement on a 45 μm sieve opening was 20%, and replacing cement with 30% of both agricultural wastes contributed to a larger Blaine-specific surface relative to traditional cement [28]. Moreover, several types of sustainable materials, such as rice husk ash (RHA) and OWA were simultaneously applied to produce high-strength concrete [29]. The substitution levels of RHA used varied from 0 to 25% with an increment of 5%, while OWA levels ranged from 0 to 7.5% with an addition of 2.5%. The tests conducted included the slump test, compressive, splitting tensile, flexural strength, modulus of elasticity, and bond strength. The outcomes emphasized that replacing cement with 20% RHA and 5% OWA significantly enhanced all the mechanical strengths due to the pozzolanic activity of these alternative materials [29]. A previous study was conducted to fabricate self-compacting concrete with two green materials such as sea sand powder (SS) and olive waste bottom ash (OW) instead of traditional filler (limestone powder) [30,31]. To investigate the effect of OW filler on the performance of concrete, different properties including compressive and tensile strengths as well as volume stability were evaluated. As a result, OW contributed to a loss in compressive strength as well as a decrease in workability; however, there was an augmentation in shrinkage values mostly associated with the high porosity [30,31]. Table 1 provides a summary of the key information from all prior studies using OWA or a combination with other SCMs.
To the best of the Authors’ knowledge, there is little information in the literature about the influence of OWA as a partial cement replacement on the volume stability of cement paste. For this purpose, five partial replacement compositions of 0, 5, 10, 15, and 20% of OWA were implemented in this research. The mechanical performance, including compressive and flexural strength, was investigated. In addition, this paper provided insights into how OWA impacted autogenous shrinkage, chemical shrinkage, drying shrinkage, and expansion. The correlations between these volumetric stability parameters were also elucidated. It is expected, at the end of this study, that the use of OWA could lead to the development of sustainable infrastructures.

2. Experimental Test

2.1. Materials

Ordinary Portland Cement CN PA-L 42.5-type obtained from Sabaa plant, Tripoli, Lebanon and OWA with a density of 950 kg/m³ were used in this work. The OWA was delivered from an olive press located in Zgharta, North Lebanon, and obtained after burning large amounts of olive residue generated from the olive oil extraction in a boiler for 8 h. The OWA was milled using a Los Angeles abrasion machine for two hours to obtain finer particles. Finally, OWA was sieved through a No. 200 sieve. A brief description of the process of olive waste ash OWA production is clarified in Figure 1. The chemical composition and the particle size distribution of OWA are shown in Table 2 and Figure 2, respectively. The chemical composition showed that OWA mainly consists of CaO (36.13%), SiO2 (24.73%), and K2O (9.56%).

2.2. Mixture Proportions

Five paste mixtures were prepared with five percentages of 0, 5, 10, 15, and 20% of OWA replacing the cement. For each type of shrinkage test (chemical, drying, autogenous shrinkage, and expansion), ten specimens were cast so the total number of specimens was forty. The water-to-cement ratio used was 0.45. Table 3 summarizes all mixture proportions and component amounts.

2.3. Testing Procedure and Specimen Preparation

2.3.1. Compressive and Flexural Strengths

To determine the compressive strength, 50 × 50 × 50 mm cubes were tested following ASTM C109 guidelines [32]. According to the flexural strength evaluation, beams of 40 × 40 × 160 mm were used as per ASTM C348 standards [33]. The data were measured at 7, 28, and 90 days.

2.3.2. Chemical Shrinkage

Chemical shrinkage was tested according to ASTM 1608 by measuring the internal volume change in cement paste due to the hydration of the cementing materials [34]. The equipment employed in this test was a graduated pipette of 2 mL, a bottle of 250 mL, a spatula, and a rubber stopper. The procedure started by placing 30 g of each mix at the bottom of the bottle corresponding to a depth of 1.8 cm. Then, the water was slowly added to the top of the matrix until the bottle was filled. The pipette was inserted into the bottle through the stopper, filled with water, and sealed at the top with a drop of oil to prevent water evaporation, as seen in Figure 3. The reading of the drop in the level of water in the pipette refers to the chemical shrinkage (change in volume) [35,36] and is computed every one hour for the first 24 h and then every two days until reaching 90 days. Two replicate samples were tested for each mix. The chemical shrinkage value was monitored by calculating the average of two readings, with the first reading considered as zero. The calculation of chemical shrinkage is expressed by the following equation:
ΔV/V = 3 ΔL/L
where ΔV = change in volume in the pipette (mL), V = initial volume of the sample (mL), ΔL = change in length in the pipette (µm), L = initial length of the sample (m).

2.3.3. Drying Shrinkage

Drying shrinkage was tested following ASTM C157 [37]. For this test, molds of 25 × 25 × 300 mm3 were used. After 24 h in the curing chamber (25 °C), the samples were demolded, and two Demec points separated by a distance of 200 mm were placed on each side of the specimen. The displacement of the Demec points was measured using a dial gauge and the length was reported every 2 days for 90 days while the specimens were in the chamber. The average of four readings from two replicated specimens refers to the drying shrinkage (change in length). The specimens are shown in Figure 4.

2.3.4. Autogenous Shrinkage

Paste specimens of 25 × 25 × 300 mm3 were tested according to ASTM C192 [38]. To record autogenous shrinkage (starting after 24 h), each specimen was immediately covered with a plastic bag as illustrated in Figure 4. After 24 h, the mean values of four readings represent the starting point (reference data). The same process for measuring the drying shrinkage records was employed for autogenous shrinkage.

2.3.5. Expansion

The specimens were cast in 25 × 25 × 300 mm3 molds. After 24 h, the formwork was removed, and each specimen was totally immersed in water at a constant temperature (20 ± 1 °C) as illustrated in Figure 5. The same procedure for monitoring the drying shrinkage data was applied for monitoring expansion as well.

3. Analysis of the Results

3.1. Compressive and Flexural Strength

The effects of OWA induced at various percentages on compressive and flexural strengths are indicated in Table 4. As can be seen from the results, as the curing time increases, there is a significant increase in compressive strength values. For example, the control mixture displays compressive strength values of 27, 47, and 50 MPa at 7, 28, and 90 days, respectively. However, the incorporation of OWA decreases these measurements independently of the amount of OWA induced. More precisely, among all mixtures containing OWA, there is a negligible loss in compressive strength in the P10% sample with a rate of 8%, displaying a magnitude of 46 MPa after 90 days of curing. Therefore, 10% of OWA can be considered as the optimal substitution level. This behavior could be attributed to the fact that the chemical composition—with 36.1% CaO and 24.7% SiO2—indicated that OWA was a cementitious material with good pozzolanic properties; this leads to the formation of additional C-S-H gel, which is the major contributor to strengthening the matrix [20,28]. Compared to the reference mixture, the decrease in compressive strength continues for the addition of 15 and 20% of OWA, achieving drops of 38 and 59%, respectively. There are two potential reasons for this: First, there was a decrease in hydrate products (C2S and C3S) resulting from the loss of cement [20,28]. Second, the higher porosity took place with the increase in OWA content [23,25].
The flexural strength results show an identical trend to the compressive strength pattern. For instance, the 90-day flexural strength is 4 MPa for the paste without OWA. The sample containing 10% of OWA displays the lowest rates of 3 and 5% after 28 and 90 days, respectively; however, this decline peaks with the addition of 20% of OWA, achieving 37%. The causes of this negative effect of OWA are as follows: first, the reduction in cement content in the matrix, and second, OWA seemed to weaken the bonding between OWA and the cement particles associated with the augmentation of the number of voids in the paste [27,29].

3.2. Chemical Shrinkage

Figure 6 depicts the results for the chemical shrinkage (μm/m) measured over 90 days. The time immediately following placement (t = 0) is considered the starting point for data collection. It is noteworthy that in the early period of curing, all curves exhibit high chemical shrinkage. Conversely, during the late ages, there is no alteration in chemical shrinkage values, which are observed in a steady state. These findings are consistent with a prior study [16]. For instance, on day 1, the chemical shrinkage for P0% was 0 μm/m, and this value rises to magnitudes of 660 and 811 μm/m at 28 and 90 days, corresponding to an increase of 23%. As previously mentioned, chemical shrinkage is referred to as the reduction in the total volume of hydrate products during the hydration process of cement. With the increase in curing time, this decrease gradually progresses during the hardening stages, thus leading to an increase in chemical shrinkage [12,13,14]. On the other hand, it is noticed that 10% of OWA partially replacing cement extremely reduces the chemical shrinkage to a measurement of 680 μm/m after 90 days of curing, showing a great reduction rate of 16%. However, the samples containing different OWA content do not show the same significant decline as observed in the sample P10%; for example, P5%, P15%, and P20% show chemical shrinkage values of 740, 750, and 780 µm/m, respectively. This slight drop is equivalent to 8, 8, and 3% compared to the control paste.
The efficiency of implementing OWA in cement paste was referred to as its potential to reduce chemical shrinkage. This effect could be mostly explained by the fact that OWA contains large amounts of SiO2, and Al2O3, indicating that OWA was likely linked to the pozzolanic activity, as stated in the literature review [21,28,39]. Therefore, the decline in chemical shrinkage could be attributed to two factors: first, the loss of cement in the paste, thereby the reduction in clinker phases responsible for chemical shrinkage occurrence; and second, the slower pozzolanic reactivity of OWA with the calcium hydroxide (CH) obtained from cement hydration. The two factors formed a combined effect in delaying the early-age hydration mechanism, therefore lowering chemical shrinkage measurements [23]. Specifically, among all mixes incorporating OWA, the mix containing 10% OWA shows the optimal reduction level as this percentage indicates a good balance between the loss of cement quantity replaced with OWA and the sufficiency of the pozzolanic reaction to continuously form hydrate products, maximizing the decrease in chemical shrinkage.

3.3. Drying Shrinkage

Figure 7 displays the drying shrinkage values of all specimens measured over 90 days. As a result, the curing time shows a major effect on the magnitude of drying shrinkage [40,41]. For example, on day 1 after placing, P5% is recorded as 0 μm/m; then, this value rises, reaching 1125 and 1850 μm/m at 28 and 90 days, respectively. Meanwhile, the drying shrinkage rises by 64% from 28 to 90 days. In addition, the drying shrinkage measurements show a logical variation with varying proportions of OWA. At lower substitution levels of 5 and 10% of OWA content, the drying shrinkage exhibits a considerable decrease, followed by a notable increase at higher levels of 15 and 20% of OWA content. For example, after 90 days, the drying shrinkage for P0% is 2015 μm/m; then, this value sharply drops to reach 1730 μm/m for 10% OWA content (P10%), achieving a decline of 14%. However, inducing higher percentages of OWA increases the drying shrinkage for samples P15% and P20% to 2275 and 2350 μm/m, representing increases of 13% and 16% over the same period, respectively.
The test results demonstrate that the drying shrinkage behaved differently in the existence of OWA [12,21]. These changes are attributed to a variety of factors like the material’s stiffness, pore structure, and internal pressures. Thus, with the addition of 5 and 10% (low levels), the pozzolanic reaction of OWA might play a significant role in decreasing this type of shrinkage. Hence, as additional C-S-H gel developed, the matrix became denser, leading to a notable reduction in porosity, meaning that less water was needed for evaporation when the paste dried, mitigating the drying shrinkage [41]. However, with the addition of 15 and 20% (high levels), OWA might incompletely compensate for the increased loss of cement amount, resulting in a rise in capillary pores, which facilitates the loss of water [1,42]. Accordingly, the high and continuous evaporation of water within the paste contributed to a reduction in the material’s stiffness and, consequently, a weakness in resisting the internal pressures caused by moisture escape, leading to an amplification of the deformation of the beam under drying conditions [17]. Furthermore, another relevant explanation for the increase in drying shrinkage could be the disjoining pressure that exists between the pores promoting the contraction of the solid body [9,22,43,44]. In light of the above outcomes, it is highly recommended to avoid using high replacement levels in the manufacturing of more durable cement-based materials, as well-demonstrated in a prior study [23]. It is inferred that the optimal percentage of cement replacement with OWA can be achieved at 10% due to its substantial effect on mitigating drying shrinkage, powerfully adequate for improving long-term durability.

3.4. Autogenous Shrinkage

The data for autogenous shrinkage of all cement pastes during 90 days are illustrated in Figure 8. As seen from the curve, there is a considerable impact of the curing time on the development of self-desiccation, particularly since all values increase as the curing time increases [45,46]. For instance, P5% shows 0 μm/m on day 1 of curing; this value rises to 600 and 950 μm/m at 28 and 90 days, respectively. In addition, incorporating OWA improves the autogenous shrinkage of the paste at various OWA content. For instance, after 90 days, P0% records the highest autogenous shrinkage value of 1125 μm/m. The inclusion of 10% of OWA content ultimately reduces autogenous shrinkage to 788 μm/m, showing a decrease of 30%. However, this drop is less pronounced with the incorporation of 15 and 20% of OWA, showing magnitudes reaching 950 and 975 µm/m, respectively. This is equivalent to a drop of 15 and 13% compared to the reference paste.
Based on the findings, as autogenous shrinkage was directly dependent on the early-age hydration mechanism, the drop in autogenous shrinkage values could be explained by the fact that the additional OWA retarded the hydration process in the early stages, lowering the magnitude of autogenous shrinkage [47,48]. In this context, the pozzolanic properties of OWA potentially slowed the reaction between OWA and CH, reducing the early-age hydration, and mitigating, by this action, the self-desiccation of the paste [20,48,49]. On the other hand, the filler effect of OWA led to the refinement of the pores, which slowed down the internal water movement into the paste, inhibiting by this behavior the development of self-desiccation as the fine particles could accommodate the voids [19,21]. It is crucial to note that OWA is an effective material in the improvement of the relative humidity, which in turn helps the mix to reduce the self-desiccation changes [3,50,51,52]. As expected, at the level of 10% OWA, there is a perfect balance between the reduced amount of cement and the suitable percentage of OWA for pozzolanic reactivity, thus controlling the porosity in a way to not be exceeded and maximizing the decrease in autogenous shrinkage. Accordingly, it is recommended to use 10% to prevent the volumetric instability resulting from autogenous shrinkage.

3.5. Expansion

Figure 9 presents the measurements for expansion of all the pastes with the varying OWA content in µm/m measured over 90 days. As displayed, all mixes show a continuous expansion along with the curing time. It can also be observed that the addition of up to 10% increases the expansion values, while inducing 15% and beyond declines the expansion. For instance, the reference mixture (P0%) has an expansion level of 2075 µm/m at 90 days. This value slightly rises for P5% and P10%, reaching 2250 and 2175 µm/m, corresponding to a growth of 8 and 5%, respectively. Then, these magnitudes drop for P15% and P20%, achieving 1900 and 1550 µm/m, respectively; this is equivalent to 9 and 25% increases relative to the control paste.
The different behavior of expansion in the presence of OWA was principally attributed to the pozzolanic reactions of OWA. For OWA content up to 10%, the expansion occurred because the amount of OWA induced was insufficient to react with CH resulting from hydration This remaining quantity of CH could subsequently react with some available constituents in OWA, contributing to the generation of expansive agents [53,54]. On the contrary, exceeding 10% of OWA content led to a further reduction in expansion measurements. This was mostly based on several reasons: First, the higher reduction in CH, the less production of expansive agents, making the paste more stable against expansion [55,56]. Second, this stability could also be the result of the filler effect of OWA, allowing it to accommodate the expansion volume [19,49]. Finally, the chemical composition of OWA also provided a reasonable indication of expansion performance. Particularly, as OWA replacement levels increase, the quantity of CaO decreases, which in turn affects the swelling of the specimens [57]. In addition, the limited quantity of SO3 present in OWA (below the 3.5% threshold) reacted with CaO to form small amounts of ettringite, which is an expansive agent, which implied expansion limitations [58,59,60]. For this reason, it was beneficial to use higher replacement levels of cement with OWA to withstand expansion, showing a pronounced decrease in swelling. In particular, among all mixes, the paste containing 20% OWA possesses the optimal percentage of replacement in terms of lowering expansion.

3.6. Relationships between Length Change Parameters

Figure 10 displays the length change parameters (drying, autogenous, chemical shrinkage, and expansion) among all mixes during the 90 days, which evolve in the early ages and are prolonged for the long term [52,61]. It appears, from the obtained results, that OWA substantially improves various types of shrinkage, which are key indicators of the durability and serviceability of cement-based materials. The magnitude of each type of volumetric stability parameter could be interpreted by the hydration process and the development of pores within the blended cement paste [47,53]. This study reveals that drying shrinkage records the highest volumetric variances compared to other types of shrinkage, reaching 2350 μm/m in the P20% sample. This was primarily caused by moisture diffusion in drying conditions and probably could last for future years after the curing of the paste [62,63,64]. This type is the best criterion for longer durability and, thereby, the lifespan of the structure [65].
Furthermore, two points can be observed in these figures: First, the chemical and autogenous shrinkage are equal in the early ages (the first few days) [45]. Second, the autogenous shrinkage values are higher than those for chemical shrinkage as time increases. For instance, at 90 days, for 5% addition, the chemical and autogenous readings are 740 and 950 μm/m, indicating a difference rate of 28%, as seen in Figure 10b. The inclusion of 10% OWA exhibits the lowest chemical and autogenous shrinkage values of 680 and 788 μm/m, respectively, as illustrated in Figure 10c. This is equivalent to a difference rate of 16%. However, the incorporation of 15% OWA raises the difference rate to 27%, as shown in Figure 10d. Similarly, the rate of difference between the chemical and autogenous shrinkage is around 25% for P20% samples, as illustrated in Figure 10e. The cause of these findings could be explained by the fact that both mechanisms are directly linked to the hydration process and occurred in the early periods [45,66,67].
To further visualize the relationships of the shrinkage performance properties, a regression equation is used to determine the coefficient of determination R2 as displayed in Figure 11, Figure 12 and Figure 13 for days 1, 7, 28, and 90. As can be seen, a positive linear correlation exists between chemical shrinkage and drying shrinkage, with a high R2 of 0.97, 0.99, 0.99, 0.97, and 0.99 for P0%, P5%, P10%, and P20%, respectively. This is because the reduction in volume resulting from the chemical reactions could induce additional internal stresses and pores, leading to higher shrinkage as the paste dries [68,69,70].
Furthermore, there is a strong dependence between chemical and autogenous shrinkage, showing a significant coefficient of correlation R2 equal to 0.96, 0.99, 0.99, 0.91, and 0.98 for P0%, P5%, P10%, P15%, and P20%, respectively. One possible explanation of this link is that chemical shrinkage can be called “internal autogenous shrinkage” while autogenous shrinkage can be referred to as “external chemical shrinkage” in some cases [63,67]. Hence, in the early stage, after reaching the stiffening point and the formation of the structure, the matrix enters the self-desiccation process due to the retention of moisture in the capillary pores; in this case, both autogenous and chemical shrinkage cannot be considered interchangeable [3,67,68].
Conversely, the expansion indicates an inverse relationship with chemical shrinkage, as evidenced by a high R2. This correlation may be interpreted to mean that the chemical shrinkage can continuously occur even if the paste is in an expansion state, especially when, in both cases, the paste is still immersed in cured water [71]. Overall, it is fundamentally justified that chemical shrinkage is the driving force for other types of shrinkage.

4. Conclusions

It is interesting to develop a sustainable management strategy to save natural resources and promote their utilization in construction. To achieve this target, olive waste ash (OWA) is used as a partial replacement for cement to test the volume stability parameters including chemical, autogenous, and drying shrinkage as well as expansion. Based on this study, several points can be outlined:
  • The presence of OWA adversely affects the mechanical properties of the pastes. For the addition of 10% OWA, the rate of reduction in both compressive and flexural strength was around 8 and 5%, respectively, compared to the control mixture. Beyond this level, at the 15 and 20% OWA levels, the compressive and flexural strengths significantly decreased, reaching 59 and 36%, respectively, for P20% samples;
  • OWA had a positive impact on chemical shrinkage. At day 90, the chemical shrinkage P0% exhibited the highest level of chemical shrinkage. However, adding 10% of OWA sharply reduced the chemical shrinkage to a rate of 16%. The drop in chemical shrinkage was found to be less pronounced for the incorporation of 15% and 20% of OWA, indicating a reduction of 8 and 3%, respectively, compared with the free OWA paste;
  • The variation in drying shrinkage depended on the percentages of OWA content. Hence, in the comparison with the control mix, the drying shrinkage ultimately decreased, reaching a rate of 14% for P10% after 90 days of curing. However, there was an increase in drying shrinkage for P15% and P20% at the rates of 13 and 16% over the same period;
  • Regarding autogenous shrinkage, there was a decrease in autogenous measurements with varying OWA content. This drop was optimal for the incorporation of 10%, showing a percentage of decline of 30%. On the other hand, this reduction was less pronounced in the P15% and P20% mixes, which exhibited decreases of 15 and 13% compared to the reference paste;
  • The expansion behaved differently with varying OWA levels. Hence, P5% and P10% exhibited a slight increase in expansion measurements, reaching rates of 8 and 5%. Contrarily, a notable decrease was observed for P15% and P20%, achieving drops of 9 and 25% relative to the control paste;
  • A positive linear relationship was observed between chemical shrinkage and drying and autogenous shrinkage. In addition, a negative linear correlation was found between chemical shrinkage and expansion. These correlations confirmed that chemical shrinkage was the driving force for the other types of shrinkage.
These conclusions suggest that olive waste ash has a substantial impact on the shrinkage and expansion of cement paste, highlighting its effectiveness as a partial replacement for cement in the development of more durable and sustainable construction materials.

Author Contributions

Conceptualization, J.K. and H.G.; methodology, S.G. and H.G.; formal analysis, S.G. and H.G.; writing—original draft preparation, S.G. and H.G.; writing—review and editing, H.G. and S.E.Z.; supervision, J.K. and A.E.; project administration, H.G. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Data Availability Statement

Data are included in this paper.

Acknowledgments

The authors express their gratitude for the assistance provided by the staff and technicians at BAU Laboratories.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Process of OWA preparation.
Figure 1. Process of OWA preparation.
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Figure 2. Particle size distribution of OWA and cement.
Figure 2. Particle size distribution of OWA and cement.
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Figure 3. (a) Chemical shrinkage setup; (b) chemical shrinkage specimens.
Figure 3. (a) Chemical shrinkage setup; (b) chemical shrinkage specimens.
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Figure 4. Specimens for (a) drying shrinkage; and (b) autogenous shrinkage.
Figure 4. Specimens for (a) drying shrinkage; and (b) autogenous shrinkage.
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Figure 5. (a) Expansion specimens; (b) strain gauge.
Figure 5. (a) Expansion specimens; (b) strain gauge.
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Figure 6. Chemical shrinkage of pastes with different levels of OWA measured over 90 days.
Figure 6. Chemical shrinkage of pastes with different levels of OWA measured over 90 days.
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Figure 7. Drying shrinkage of pastes with different levels of OWA measured over 90 days.
Figure 7. Drying shrinkage of pastes with different levels of OWA measured over 90 days.
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Figure 8. Autogenous shrinkage of pastes with different levels of OWA measured over 90 days.
Figure 8. Autogenous shrinkage of pastes with different levels of OWA measured over 90 days.
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Figure 9. Expansion of pastes with different levels of OWA measured over 90 days.
Figure 9. Expansion of pastes with different levels of OWA measured over 90 days.
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Figure 10. Length change in pastes containing (a) 0% OWA; (b) 5% OWA; (c) 10% OWA; (d) 15% OWA; (e) 20% OWA.
Figure 10. Length change in pastes containing (a) 0% OWA; (b) 5% OWA; (c) 10% OWA; (d) 15% OWA; (e) 20% OWA.
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Figure 11. Correlation between drying and chemical shrinkage for all levels of OWA.
Figure 11. Correlation between drying and chemical shrinkage for all levels of OWA.
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Figure 12. Correlation between autogenous and chemical shrinkage for all levels of OWA.
Figure 12. Correlation between autogenous and chemical shrinkage for all levels of OWA.
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Figure 13. Correlation between expansion and chemical shrinkage for all levels of OWA.
Figure 13. Correlation between expansion and chemical shrinkage for all levels of OWA.
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Table 1. Summary of previous studies using OWA with/without other SCMs.
Table 1. Summary of previous studies using OWA with/without other SCMs.
ReferencesMaterials (%)Tests ConductedResults
[21]OWA (0, 3, and 6%) replacing natural sand-Drying shrinkage for non-structural recycled concrete-Higher drying shrinkage
[22]OWA (0 to 15% with a constant addition of 3%) replacing cement-Setting time
-Expansion for cement paste		-Increase in setting time, thus, retarded hydration
-Gradual decrease in expansion values with increasing OWA content
[23]BBA replacing cement -Drying shrinkage for mortar-High dimensional changes related to the increased porosity
[25]OPBA (0, 5, 10, 15, and 20% by weight)For clay bricks:
-Bulk density
-Linear shrinkage
-Water absorption
-Porosity
-Compressive strength
-Thermal conductivity		-Greater compressive strength in the sample with 5% of OPBA (11.5 MPa)
-Highest linear shrinkage and porosity as well as lowest density for 20% OPBA sample
-Best thermal insulation
[26]BBA (0, 15, 50, and 100%)In soil stabilization for road embankment-Enhancement in mechanical properties
-Reduction in soil expansion
[27]-BBA (0, 10, and 20%) replacing cement and natural sand
-Two types of cement (CEM-Ⅰ and CEM-Ⅱ)
-amount of cement (515, 485, and 450 g/L		For mortars:
-Compressive strength
-Flexural strength
-Density
-Porosity		-Decline in the mechanical properties
-Decrease in density and porosity due to high water absorption of BBA
[28]Olive pomace and olive kernel replacing cement with 10 and 30% by massFor cement mortars:
-Compressive strength
-influence of particle size
-Heat evolution
-Setting time		-Similar compressive strength to that of the control mixture
-After two hours of milling, a larger Blaine-specific surface relative to traditional cement with the addition of 30% of pomace and olive kernel
-Greater heat evolution and hydration
[29]-OWA (0, 2.5, 5, and 7.5%) replacing cement
-RHA (0, 5, 10, 15, 20, and 25%) replacing cement		For high-strength concrete:
-Slump test
-Compressive strength
-Splitting tensile strength
-Flexural strength
-Modulus of elasticity
-Bond strength		-Decrease in slump records and workability
-Increase in compressive strength by 58% for replacements of 20% RHA with 5% OWA
-Improvement in all mechanical strengths due to the pozzolanic activity of these ashes
-Larger surface areas of binder, thus, leading to high water absorption
-Lower amount of pores related to the densification of the matrix
[30,31]-SS filler (10 and 15% of total aggregate content)
-OW filler (5, 10, and 15% of total aggregate content)		-Compressive strength
-Volume stability		-Detrimental effect on workability and compressive strength
-Increase in volumetric shrinkage and porosity
-The usage of OW must be less than 5%
-No segregation and bleeding in OW mixes
Table 2. Chemical composition of OWA and cement.
Table 2. Chemical composition of OWA and cement.
OxideSiO2Al2O3Fe2O3CaOMgOSO3K2ONa2OLOIOther
OWA24.733.413.8336.132.810.039.561.4214.73.38
Cement18.533.933.0661.781.742.920.470.186.31.09
Table 3. Mix proportions and component quantities of paste.
Table 3. Mix proportions and component quantities of paste.
ProportionsAmount (kg/m³)
Paste CodeCementOWAW/C RatioCementOWAWater
P0%100.451303.50.0586.2
P5%0.950.050.451260.066.2566.9
P10%0.90.10.451215.1134.7546.9
P15%0.850.150.451168.5205.6526.2
P20%0.80.20.451120.1280.6504.1
Table 4. Compressive and flexural strengths of all cement pastes.
Table 4. Compressive and flexural strengths of all cement pastes.
PasteCompressive Strength (MPa)Flexural Strength (MPa)
7 Days28 Days90 Days7 Days28 Days90 Days
P0%27.247502.63.74
P5%2331.532.22.43.43.6
P10%25.442.545.42.53.63.8
P15%2328.7312.32.62.8
P20%14.418.920.322.32.5
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Ghazzawi, S.; Ghanem, H.; Khatib, J.; El Zahab, S.; Elkordi, A. Effect of Olive Waste Ash as a Partial Replacement of Cement on the Volume Stability of Cement Paste. Infrastructures 2024, 9, 193. https://doi.org/10.3390/infrastructures9110193

AMA Style

Ghazzawi S, Ghanem H, Khatib J, El Zahab S, Elkordi A. Effect of Olive Waste Ash as a Partial Replacement of Cement on the Volume Stability of Cement Paste. Infrastructures. 2024; 9(11):193. https://doi.org/10.3390/infrastructures9110193

Chicago/Turabian Style

Ghazzawi, Safa, Hassan Ghanem, Jamal Khatib, Samer El Zahab, and Adel Elkordi. 2024. "Effect of Olive Waste Ash as a Partial Replacement of Cement on the Volume Stability of Cement Paste" Infrastructures 9, no. 11: 193. https://doi.org/10.3390/infrastructures9110193

APA Style

Ghazzawi, S., Ghanem, H., Khatib, J., El Zahab, S., & Elkordi, A. (2024). Effect of Olive Waste Ash as a Partial Replacement of Cement on the Volume Stability of Cement Paste. Infrastructures, 9(11), 193. https://doi.org/10.3390/infrastructures9110193

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