The influence of selected grain size fractions of coal fly ash on properties of clay-cement mortars used for the flood levees construction | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article The influence of selected grain size fractions of coal fly ash on properties of clay-cement mortars used for the flood levees construction Jurij Delihowski, Piotr Izak, Łukasz Wójcik, Agata Stempkowska, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4100023/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 14 Sep, 2024 Read the published version in Scientific Reports → Version 1 posted 10 You are reading this latest preprint version Abstract This study examines the influence of different grain size fractions of coal fly ash on the properties of clay-cement mortars used in flood levee construction. Dry aerodynamic separation and mesh sieving were employed to obtain ultra-fine, fine, and medium fractions of high-calcium and silicious fly ash. The experimental results reveal that the rheological properties of fresh mortars are significantly influenced by these fractions. High-calcium fly ash mortars exhibit high reactivity and rapid viscosity increase, with finer fractions showing the highest reactivity. Silica ashes show increased reactivity in the later stages of suspension hardening. Their spherical shape contributes to reducing internal friction during flow in initial technological operations. Furthermore, the compressive strength of hardened mortars improves as the particle size decreases for both ashes resulting in dense and uniform microstructure. The separation and fractionation of fly ashes contribute to obtaining fractions that influence clay-cement suspension application parameters at different scales. Results show the potential benefits of the separation of ash which can bring advantages in terms of economic viability, engineering performance, and ecological sustainability. Physical sciences/Engineering/Civil engineering Physical sciences/Engineering/Mechanical engineering clay-cement suspensions coal fly ash compressive strain particle size distribution and properties rheology Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 HIGHLIGHTS - The grain fractions of ash affect the rheological properties and mechanical strength of barriers that are used in flood control applications. - Fractionation has a significant impact on structure formation intensity , hydration processes and grain reactivity. -The increase in viscosity immediately after mixing and its effect on the workability of fly ash mixtures for barriers depends primarily on the development of the surface, that is, directly on the size of the particles 1. Introduction Coal combustion for energy purposes generates combustion by-products, where fly ash constitutes up to 70-90% of the total by-products [1,2]. Fly ash consists of incompletely burned organic residues and thermally transformed mineral matter present in feedcoal. Pounds and disposals, where those ashes are stored, occupy large natural territories and can have a harmful impact on surrounding areas, underground water, and the atmosphere [3–6]. Globally, fly ash utilization rates vary: India used 66% of its 233 million tons in 2021 [7], China applied most of its 550 million tons produced in 2018 to construction and cement [8], Australia utilized 47% of 14 million tons in 2019 [9], and Europe used a significant portion of over 1 billion tons produced from 1965 to 2015 in cement and road construction [10]. While some countries achieve 100% utilization, the average global rate is around 60% [11]. Due to the necessity of utilizing incredible amounts of those by-products, numerous applications across various industrial sectors have incorporated fly ashes into production processes. Some examples include its use in ceramics, composite engineering, the cement industry, and soil modification and stabilization additives [4,6,12,13]. Mineralogical and chemical characteristics of fly ash can vary significantly depending on such factors as coal type and origin, combustion process, and precipitation techniques [2,3,14]. A better understanding of tendencies and variations in fly ash properties can help to design efficient utilization strategies and incorporate ashes in new industries. Fly ash processing and separation are commonly used for enhancing ash properties and extracting various grain fractions with desired parameters [3,4]. Concerning this study, the separation due to the grain size will be briefly discussed. In general, fine-grained fractions are associated with increased levels of certain phases, e.g. alumo- and calcium-silicates. These phases are known to be important for the pozzolanic properties of fly ash, which enhance the strength and durability of concrete [15–17]. In terms of chemical composition, those fine ash fractions tend to be enriched in certain oxides, e.g. sulphur, chlorine, and potassium as well as some trace elements, e.g. Mn, Mg, Zn, Cr, Ni and Pb [4]. Middle-sized and coarse fractions generally have different mineralogical and chemical characteristics compared to fine fractions [3,15]. Coarse fractions tend to be enriched in crystalline phases, including significant levels of mullite and quartz as well as unburned feedcoal grains. These mineral grains can act as supplementary inert unreactive fillers in constructions and concrete. By subjecting coarse fractions to additional pretreatment (mechanical, chemical, or thermal), their reactive potential can be activated, which in turn, transforms them into active pozzolanic additives [18–21]. Middle-sized fractions are also known to have some pozzolanic properties [22,23]. The chemical composition of middle-sized fractions generally contains lower levels of active elements compared to fine fractions and a higher amount of amorphous fractions compared to a coarse fraction. Worth, noticing is a high level of porosity and the highest level of presence of cenospheres in this fraction [24–26]. This can make them a more attractive option for certain specific applications where some restrictions to building materials are required, e.g. lightweight building materials, thermal insulators, etc [6,12,13]. Among many other applications, fly ash has become a popular filler material for hydraulic structures and, in particular, clay-cement suspensions for flood-levees construction [27,28]. Those sealing suspensions consist of base clay-water suspension and cement, forming a thixotropic fluid that can be pumped and introduced into embankments, gaining strength over time. They provide the necessary strength, stability, and water resistance for levees. In these suspensions, clay provides cohesive and impermeable properties, while the cement acts as a binder that improves strength in the later stages of curing. The interactions between the clay platelets, cement hydration products and water create a complex microstructure resembling a continuous 3D network with mechanical durability and infiltration properties [29–31]. Fly ash additives can influence this network in several ways. The reactions between clay minerals, cement and fly ash modifies the fresh mortars rheology and further microstructural development during the curing stages. The fly ash particles are capable of filling voids, enhancing packing density, and increasing infiltration properties. Moreover, the increased surface area of ashes offers additional sites for hydration and pozzolanic reactions. In addition, fly ash additives can improve chemical resistance and as a result, increase the durability and safety of structures [28,30–32]. In this study, the influence of selected fly ash fractions on the properties of clay-cement sealing suspensions used for flood levees was investigated. The influence of the addition of different grain size fractions on rheological properties and compressive strength was examined and discussed. The results can contribute to a better understanding of the possibilities of using selected ash fractions and their impact on the properties of final products. 2. Materials and methods 2.1 Materials Fly ash Two different types of fly ashes from Polish power plants were used: S1 – High calcareous fly ash from lignite combustion (S1.O), obtained from Belchatów power plant, Poland, from the combustion of brown coal. S2 – Silicious fly ash from bituminous coal (S2.O), from Kraków power plant, Poland. Granulometric separation was used to obtain representative fractions. The chemical, mineralogical, and granulometric composition of obtained fractions is presented in the following parts. Cement The Cement CEM I 42.5 R Odra Opole, produced by Cement plant "Odra" S.A., is composed of Portland clinker in the range of 95-100% and secondary components such as gypsum in the range of 0-5%. The chemical composition is presented in Table 1. Table 1. Chemical composition of Cement CEM I 42,5 R Odra Opole Chemical composition (%wt.) SiO 2 Al 2 O 3 Fe 2 O 3 CaO MgO Na 2 O eq 19.8 6.2 2.6 63 1.4 0.6 Clay The mineral accompanying the brown coal deposits in the Bełchatów mine was used as the clay raw material. The Bełchatów clay present in this paper is the most common clayey silt in this deposit. Chemical composition is presented at Table 2. Table 2. Chemical composition of Clay Bełchatów Chemical composition (%wt.) SiO 2 Al 2 O 3 CaO MgO Fe 2 O 3 MnO Na 2 O K 2 O TiO 2 H 2 O LOI 58.65 14.55 4.75 0.72 3.46 0.72 1.02 1.05 0.42 5.52 9.72 From a mineralogical point of view, this clay consists mainly of beidellite and quartz 2.2. Methods Chemical composition analysis XRF The WD-XRF spectrometer S8 TIGER from Bruker was used for the analysis. The measurements were performed using the vacuum method with the built-in Quant Express reference standard. Mineralogical analysis XRD The phase composition of the ashes was determined using a PANalytical Empyrean X-ray diffractometer. The measurements were performed using monochromatic radiation with a wavelength corresponding to the copper K(α1) emission line (1.54178 Å), in the angular range of 5-90 degrees in 2θ scale, with a goniometer step size of 0.008 degrees. The qualitative analysis of the phase composition was carried out using the X'Pert HighScore Plus computer program developed by PANalytical. The reference databases: PDF-2 (2004) and ICSD Database FIZ Karlsruhe (2012). Lost of ignitions (LOI) LOI tests were performed according to the ASTM D7348 procedure. In the first step, the sample was weighted and heated at 110 ̊C for 1 hour. Then, the sample was placed in a desiccator to cool for 60 min before being reweighted. The weight loss in this step was recorded as moisture content. In the second step, dried fly ash was placed in a furnace and heated in a stepped schedule for 2 hr to reach 950 ̊C. The fired sample was cooled down to room temperature in a desiccator and then weighted. The weight loss associated with firing the sample is known as the loss of ignition (LOI). Density analysis Density analysis was performed using the volumetric method in a discontinuous manner with the Micromeritics ASAP 2010. The sample was degassed at 350C for 24 hours under a vacuum of 10-3 mmHg. The BET multi-point method was used to determine the specific surface area at relative pressures ranging from 0.05 to 0.30. Volume calibration was performed by the apparatus before the actual measurement. Nitrogen with a purity of 99.999% was used as the adsorbate, and the measurement was conducted at the temperature of liquid nitrogen. Rheological measurements For the rheological studies, a Brookfield DV-III+ rheometer with a coaxial cylinder system was used, which allows for the measurement of shear stress or viscosity of liquids at different shear rates. The first part of the rheological investigation focused on studying the short-time reactivity of fly ashes, both S1 and S2, and their fractions. The tests were performed using water-fly ash suspensions, where the ash-to-water ratio was adjusted (w/a). For S1 fly ashes, w/a ratio was set at 10/3, and for S2 fly ashes at 1/1. These ratios were chosen based on noticeable differences in water demand and the suspensions' workability, with S1 ashes exhibiting greater reactivity compared to S2 ashes. The measurement was performed at a constant shear rate of 20 rpm immediately after suspension preparation. The test duration time was 40 minutes. Obtained changes in suspension viscosity provided insights into the short-time reactivity of the fly ashes, concerning their ability to react with water immediately after mixing and their ability to form a spatial structure. Results of the short-time reactivity of fly ashes are presented in Figure 3. The second part of the rheological tests involved measuring the rheological properties of various fly ash–clay-cement mixtures. The viscosity measurements were conducted using an algorithm where the shear rate was incremented by 2.0 rpm every 30 seconds. The rheometer started at 2.0 rpm and the data at each speed change was collected, up to a maximum of 40.0 rpm. Then, a second stage of measurements takes place, and the shear rate decreases until reaching 2.0 rpm. For each data point the apparent viscosity, shear stress, and time were measured. Mixtures were prepared for the 20%, 30% and 40% fly ash additives by weight. Where for S1 ashes the base suspension density of 1.13 g/cm 3 was selected, and for S2 ashes 1.20g/cm 3 . Cement in all mixtures states 10% by weight. Such recipes allow for the most appropriate measurement. Results for the rheological properties of various fly ash-clay-cement mixtures are presented in Figure 4 and Figure 5. Mechanical measurements The compressive strain tests were conducted using the ZwickRoell Tira Test 2300 mechanical testing machine with Senga software. Cylindrical samples measured 45x45mm were subjected to a curing process submerged in water and were tested after 14, 28, and 90 days of curing. SEM and microstructure Scanning Electron Microscopy (SEM): Measurements were performed on the obtained fly ash fractions and hardened mortars after 14, 28, and 90 days of curing. The Thermoscientific Fisher Phenom XL SEM equipped with an Energy Dispersive Spectroscopy (EDS) attachment was used. The EDS attachment allows for the efficient determination of the point chemical composition of the tested samples 3. Results & Discussion 3.1. Fly ash fractions characteristic Granulometry and microstructure characteristic The dry aerodynamic separation process resulted in the obtaining of different fractions based on the grain size distribution. The ACX separator produced by COMEX Polska sp.zoo. was used [33]. These fractions include: Ultra Fine fraction (UF): particles with a grain size range of 0 to 10 μm. It consists of the finest obtained particles. Fine fraction (F) has a grain size distribution from around 5 to 20 μm. This fraction contains particles slightly larger than those in the UF fraction. Middle fraction (M) was obtained through manual sieving of the residues from aerodynamic separation by using a 100 μm mesh sieve, resulting in grain size range from approx. 20 to 100 μm, and represents particles of intermediate range size. Coarse fraction (C) mainly consists of grains larger than 100 μm and represents the residues on top of the 100 μm sieve. The d 90 , d 50 and d 10 parameters in Table 3. were used to determine fractions size, representing percentiles denoted by the letter d followed by the % value. Thus, d 10 = 1.7µm means that 10% of the particles are smaller than 1.7µm, etc. Figure 1 presents the granulometric distribution of obtained fractions as a cumulative volume chart. Table 3. Fly ash fractions granulometry S1.O S1.C S1.M S1.F S1.UF S2.O S2.C S2.M S2.F S2.UF Distribution (μm) d 10 1.7 69.6 22.7 1.17 0.5 3.1 73.8 17.6 1.8 0.4 d 50 28.4 159.7 53.6 7.4 2.3 21.9 179.2 52.3 5.9 2.4 d 90 140.3 349.8 101.8 19.9 9.8 142.6 338 102.6 21.2 10.5 Chemical and mineralogical composition The chemical composition of obtained fractions for S1 and S2 ashes is presented in Table 4. Table 4. Chemical composition of S1 and S2 fly ash fractions Chemical composition (% wt) S1.O S1.C S1.M S1.F S1.UF S2.O S2.C S2.M S2.F S2.UF SiO 2 30.9 44.4 28.8 21.1 16.2 54.2 58.9 51.3 49.7 48.0 Al 2 O 3 30.1 33.1 28.8 26.0 24.1 24.5 23.7 23.0 29.5 30.1 CaO 24.7 12.5 25.4 33.9 37.8 5.1 3.0 6.6 4.3 4.2 SO 3 0.2 2.1 3.4 4.7 6.4 0.4 0.3 0.4 1.0 1.3 Fe 2 O 3 9.5 5.7 10.7 10.6 10.4 8.3 7.0 9.1 6.1 5.9 MgO 1.1 0.8 1.0 1.3 1.5 3.4 2.5 4.2 2.9 2.5 TiO 2 0.7 0.9 0.7 0.6 0.6 1.0 0.9 0.9 1.3 1.3 P 2 O 5 0.6 0.4 0.6 0.5 0.6 0.3 0.2 0.3 0.7 0.9 K 2 O 0.2 0.2 0.1 0.1 0.2 2.6 2.7 2.6 3.3 3.2 Na 2 O - - - - - 1.0 0.6 1.5 2.3 2.4 Total Ʃ 98.0 100.1 99.5 98.8 97.8 100.8 99.8 99.9 101.1 99.8 LOI (% of total mass) 1.7 6.5 0.9 1.7 1.8 11.2 14.9 7.7 13.3 13.3 The mineralogical composition is presented in Tables 5 and Table 6. The identified phases in each fraction are denoted using a ranking scale to indicate the relative abundance: "-" indicates the absence or very low phase presence; "+" denotes a minor amount of the phase; "++" signifies the phase presence in moderate quantities; "+++" represents a high amount of the phase compared to other fractions. In Figure 2 density and obtained surface area of fractions are presented. Table 5. Mineralogical composition of S1 ash fractions Identified phase S1.O S1.C S1.M S1.F S1.UF Calcite - - - + + Eckermannite- gehlenite ++ + ++ ++ ++ Quarts low + ++ ++ - - Anhydrite + - + ++ +++ Hematite + - + ++ + Mullite - + - - - Lime - - - - + Complex high-calcium oxides + - ++ +++ +++ Amorphous ++ ++ ++ ++ ++ Table 6. Mineralogical composition of S2 ash fractions Identified phase S2.O S2.C S2.M S2.F S2.UF Calcite - - - + - Mullite ++ + ++ ++ ++ Quartz low ++ ++ ++ + + Hematite + - + + + Lime - - + - - Amorphous ++ ++ ++ +++ +++ The X-ray diffraction analysis of S1 fly ash samples highlights a variety of complex high-calcium oxides with increasing concentrations in finer fractions S1.F and S1.UF. Those are calcium sodium aluminum oxide, calcium aluminum oxide sulfate, calcium iron aluminum oxide, and calcium magnesium aluminum silicate. These oxides are characterized by structurally modified forms with variable chemical compositions, which also affects their reactivity. Compounds involving calcium, aluminum, and sulfate ions can participate in various chemical reactions when exposed to water. For instance, calcium sodium aluminum oxide might form aluminum hydroxide and sodium hydroxide, releasing heat in the process when exposed to water. Calcium aluminum oxide sulfate is the anhydrite/gypsum-like phase that can undergo relatively rapid surface hydration reactions with water, increasing viscosity. The presence of these minerals in finer fractions suggests quicker hydration reactions due to larger surface areas and fineness of grains [34–38]. Worth noticing, that the mineral distribution across grain sizes in fly ashes indicates a "disintegration effect"[39,40]. Hard minerals like quartz, show a lower tendency to be affected by mechanical separation, typically remaining in the coarser fractions. Conversely, softer minerals like anhydrite appear more frequently in the finer fractions, due to their greater susceptibility to breakdown during processing. Such low-durable minerals concentrated in fine fractions strongly influence short-time reactivity thus causing viscosity increase. Gehlenite, a mineral containing calcium and silica, can react with water and contribute to a rapid viscosity increase in the suspension. Anhydrite can interact with water to form gypsum and the potential formation of ettringite from calcium aluminum oxide sulfate. The S1 fly ashes contain an increased amount of these and other compounds, which are unevenly distributed throughout the particle size range, contributing to the difference in reactivity among the fractions (Tab.4) [41–45]. The observed mineralogical distribution finds a response in the chemical composition results of fly ash samples S1 and S2, with a focus on their finer fractions, suggesting that the alumosilicate glass present is likely to exhibit higher levels of modification compared to the coarser fractions [38,46]. In finer fractions, the glass phase is expected to be less siliceous and more modified, potentially enriched with network modifiers like calcium, magnesium, sodium, and potassium, as in accordance with the results of the chemical composition analysis. These modifiers disrupt the glass structure, making it more reactive. This contrasts with the coarser fractions, where the glass is anticipated to be more siliceous and less modified, thus more stable and slower in participating in pozzolanic reactions. The composition of the glass phase, including the balance of network formers and modifiers, plays a critical role in the reactivity of the fly ash, influencing the dissolution rates and the formation of strength-enhancing products within the cement matrix. 3.2. Rheological Tests Short-time reactivity For both ashes in water suspensions (Fig.3), the viscosity increase with a measure of time was observed. This suggests that some ash-water reactions start immediately after mixing. The S1 ashes, with their higher calcium content, demonstrate faster reactivity, while the more siliceous nature of S2 results in slower reactivity. Notably, the coarse S1.C fraction, despite having less reactive mineral composition than the S1.UF and S1.F groups show a tendency for quicker viscosity development in the initial stage (2-3 minutes). This behavior can be attributed to the presence of large angular particles which results in interlocking and/or rapid sedimentation of the coarse grains, resulting in a shear-thinning behavior similar to that of sand [47]. However, it is observed that the viscosity increases in fine S1.F and S1.UF fractions are lower compared to S1.M fraction (Fig.3(a)). This can be explained by the dominant factor influencing the viscosity increase immediately after mixing for these ashes being the surface area development and thus free water absorption. The S1.M fraction has the highest surface development compared to the other fractions, stating 67 m 2 /g, resulting in the absorption of free water and an accompanying viscosity increase, while for S1.UF and S1.F states 13.1 m 2 /g and 8.2 m 2 /g (Fig.2). For all S1 samples, the system stabilizes within 15 to 30 min after mixing ensuring the stability of the rheological measurements at a constant level. Stabilization refers to the equilibrium of the phenomena of structure formation and shear-thinning structure destruction. For S2 ash fractions, the highest viscosity increase rate is observed for S2.C coarse fraction. Similarly to S1.C fraction, this can be related to sedimentation and interlocking effects of coarse angular grains. Medium S2.M fraction shows very similar characteristics to the original S2.O ash with a slight viscosity increase after the 25th minute of measurement which can suggest at the starting of hydration reactions—the ultrafine S2.UF fraction does not show reactivity ability as it was in S1.F and S1.UF fine fractions. Furthermore, the high spherical S2.F and S2.UF ashes cause a decrease in suspension viscosity compared to the original ash S2.O, probably due to the ball-bearing effect [48–50]. Generally, due to the relatively high Si-Al composition and low Ca-compounds of S2 bituminous ashes, a low level of short-time reactivity is observed. In summary, the increase in viscosity immediately after mixing and its impact on the workability of the fly ash mixtures is primarily influenced by surface development and water absorption. Secondary influences have the presence of reactive minerals and compounds, as well as the shape of the individual particles. The presence of spherical grains results in a reduction of internal friction, while coarse angular fractions cause an interlocking thickening effect. However, further analysis would be required to fully understand all the processes influencing the viscosity changes and setting of the water-ash suspensions. Sealing suspensions rheology The figures in this chapter present a sealing suspension viscosity change as a function of the shear rate. The solid-filled markers present the part of the measurement for increasing shear rate speeds, and no-filled markers – for the decreasing shear rates. Figure 4 presents the comparison between S1.O, S1.UF and S2.O, S2.UF samples with identical suspension proportions: fly ash 20%, cement 10%, base suspension density 1.20g/cm 3 . Course fractions C, due to the large grains, provide significant distortions to rheological measurement results, making them meaningless and causing a high probability of damaging the equipment. For those reasons, Coarse fraction studies were limited in this work. The S1 ashes, due to their high reactivity, show a fast viscosity increase. The S1.O sample shows shear thickening characteristics [47,51]. Addition 20% of high reactive S1.UF fraction to the 1.20g/cm 3 dense suspension results in the extension of a measurement scope after the first measuring point. Therefore, in further measurements for S1 ashes samples, to obtain sufficient workability, the base suspension density of 1.13g/cm 3 was used. The less reactive S2 ashes demonstrate the shear thinning behavior, whereas curves for decreasing share rates lay lower than for increasing share rates. The S2.UF fraction additive shows an increase in viscosity compared to the S2.O fraction, which is inconsistent with the results from the previous section (Fig.3). It can be probably related to clay particles in suspensions which block or reduce the friction-thinning ball-bearing effect of the ash grains. This also indicates that the behavior of fly ash fractions differs when tested in pure water as compared to when tested in a clay-water suspension. Fly Ash granulometry influence Fine fractions S1.F and S1.UF shows the behavior according to expectations and cases of fast viscosity increase after mixing (Fig.5). The reduction of S1 fly ash particle size cases in an increase in the viscosity of clay-cement suspensions. In the high shear rate region, the balance between suspension structure formation and destruction is obtained. At lower shear rates area, an increase in stress can be observed due to faster structure rebuilding, leading to an increase in viscosity. For S1.UF suspension the viscosity acquires values beyond the measurement range at a shear rate of 20 rpm. Similarly, the S1.F fraction results in a constant increase of viscosity followed by an exceeding of scope. It is worth noting that for the S1.M fraction, based on ash-water reactivity results (Fig.3), the highest viscosity development in clay-cementitious suspension was expected. However, the S1.M viscosity behavior is not consistent with those expectations, and the obtained results remain relatively low in a whole range of measurements. This indicates that the S1.M ash does not possess reactive properties to the same extent as the S1.UF and S1.F fractions and the described viscosity increase in S1.M water suspension (Fig.3) were mainly caused by the absorption of free water in fly ash surfaces. Meanwhile, in the case of clay-based suspensions (Fig.5), a relatively low viscosity level may be attributed to the following factors: Clay particles form a layer on the surface of the fly ash, acting as a surface agent and blocking water molecules' access to the ash surface. This layer can act as a barrier, preventing water from reaching pores, voids, and cracks on the ash surface where it could be adsorbed. This hinders the water absorption process so more free water stays in suspension and viscosity stays relatively low [52]; Clay particles can form aggregates and structural networks in water-clay suspensions, phenomena related to this ability are well-studied in literature [47,52,53]. These structures can block the movement of water molecules, reducing the availability of adsorption sites on the fly ash surface. This also slows down the water absorption by ash; Clay particles contribute the ability to water absorption on their surface and by their internal structure. If clay particles are present in a high concentration in a clay-water suspension, they can adsorb water, competing with fly ash. This can reduce the available surface area for water adsorption by fly ash particles, as water molecules are bound to clay minerals so maintaining free water in suspension and enhancing flowability etc.[54–56] For the S2 ashes, the addition of S2.F fraction allows for a viscosity reduction compared to both S2.M and S2.UF fractions. This can be related to the interaction between clay particles and ash grains, where S2.F grains are large enough to cause a ball-bearing effect and reduce suspension internal friction. While for F2.UF ultra-fine grains, the clay particles can cover ash surfaces and block their ball-bearing behavior which causes the suspension viscosity to increase. For coarser F2.M fraction, as was expected according to short-time reactivity results from Figure 3, the suspension viscosity reached the highest values. The addition of obtained fractions case in increasing suspension viscosity compared to S2.O original ashes. 3.3. Compressive strain and microstructure analysis results Compressive strain results In to the base clay-water suspension with a density of 1.13g/cm 3 for S1 ashes and 1.20g/cm 3 for S2 ashes, the 10% of cement and the 20%, 30%, and 40%wt of individual fly ash fractions were added and mixed. Differences in base suspension density are related to the workability of fresh mixtures. The results of comprehensive strain tests at 14, 28, and 90 days of underwater curing are presented in Figure 6. The obtained results show that decreasing the fineness of fly ash fractions increased obtained compressive strength for both S1 and S2 ashes, resulting at 2.48, 2.65, 2.97, 4.70 and 6.93 MPa for S1.O, S1.C, S1.M, S1.F and S1.UF 40%; and 4.46, 1.71, 4.30, 5.75 and 5.95 MPa for S1.O, S2.C, S2.M, S2.F and S2.UF 40% samples respectively. The 40% ultrafine fraction S1.UF additive gave the maximum obtained strain of tasted recipes showing approx. 179% strain improvement compared to S1.O original ash, while for S2.UF 40% sample this improvement states approx. 33% compared to S2.O. These strain improvements can be attributed to several factors among which is the chemical and mineralogical composition of fractions with a higher concentration of reactive mineral phases in the finer fractions. In addition, particle fineness promotes more active participation of grains in structure-forming reactions due to the increased contact between the particle surfaces and water, compared to coarser grains. On the other hand, the particle size of F and UF fractions influences suspension workability and structure arrangement. As a result, the denser and more compact microstructure is formed, with individual grains undergoing a more extensive reaction. This reduction in porosity and enhanced interaction contributes significantly to the compressive strain development. Microstructure analysis confirms that coarse grain addition causes the formation of a structure with large pores and cracks, while fine fractions result in a dense uniform structure. Figure 8 shows the influence of particle size on the microstructure formations. For both ashes, there is a noticeable intensification of strain gain at later stages, which is consistent with the theory of delayed reactions in fly ashes [16,23,57]. Worth noticing is the variance in base suspension densities used to achieve the optimal workability of mixtures, with S1 ashes having a density of 1.13 g/cm³ and S2 ashes at 1.20 g/cm³. Due to this difference, direct comparisons of the two ash types at the same replacement levels based on module values of final strain results are not appropriate. However, an analysis of the nature of strength development over time can be performed: S1 ashes showed faster early compressive strain development in the 14-28 day period followed by slower later-stage strain gain compared to S2 ashes. S2 ashes instead had low initial strength gain but higher late-stage strength increased between 28-90 days. This could be attributed to the highly reactive mineralogical compounds in S1 lignite ashes that react at an early stage period, while for less reactive S2 bituminous ashes those structure-forming reactions are shifted to later stages of curing. This can also be observed in SEM images Figure 7 and Figure 9 and will be partly discussed in further chapter. While the coarser particles (C fraction) understandably had lower overall reactivity, especially at early stages, the strong initial strain development at 0-14 days can be observed for both S1.C and S2.C ashes. This can be related to the interlocking effect, where the angular shape of the Coarse grains contributes to mechanical interlocking between particles which manifested as reasonably high early strain test results [17,58,59] The medium fractions for both ash types S1.M and S2.M showed the overall lowest strength values, possibly because these particles were not large enough for a significant interlocking effect for the early-stage compressive strain gain, nor fine enough to contain sufficient reactive potential as in F and UF fractions. In addition, for the S2 ashes, the interlocking effect influence on structure-forming processes is lower compared to S1, due to the nature of grains shape which is predominantly spherical and smooth for S2 bituminous ashes. Bituminous coal combustion processes take place at higher temperatures which results in an increase in the amount of melted particles and a higher average smoothness and sphericity of grains [24,25]. Increasing the amount of ash additives beyond a certain limit may negatively impact the final strain results. This negative effect may appear due to the absorption of free water essential for the hydration microstructure formation processes, however, curing in underwater conditions might eliminate this factor. Furthermore, increased ash content can result in a loss of workability, as was confirmed by rheological tests, leading to an insufficient settling of fresh mortars and incomplete structural continuity promoting the formation of cracks, pores, and internal stresses. Additionally, excessive ash content in the matrix can result in increasing non-reactive ash-to-ash interconnection clusters which impede strain development (Fig.6), particularly in the early stages when coarse particles are involved [60,61]. This effect can be observed in S2.C samples, where 40% ash addition results in a decrease of final strain compared to S2.C 30% resulting at 2.85 MPa and 1.71 MPa resp. For individual fly ash types and fractions, it is important to adjust the quantities and composition of additives to achieve the desired outcomes, as they may exhibit varying behaviors, leading to different results. Fly Ash granulometry influence The microstructural studies sustain the compressive strain results, and there was a strong correlation observed between the obtained strain and microstructural results. Comparative analysis of the microscopic morphology (Fig.7, Fig.9, Fig.10) demonstrates that in the early period of 14 days, the spherical fly ash particles were still smooth, which indicates their relatively longer time reactivity, compared to high Ca-content grains and cement particles. The fly ash particles began to hydrate from the surface at later stages, so at 28 and 90 days the pits in the inert surface can be observed. Worth noticing is the lower particle dissolution level of S2 ashes compared to S1. This can be related to the higher Si content of S2 ashes, so those particles have longer activation and dissolution time. Figure 9 presents the reactivity rate of ashes at 90 days of curing depending on the EDS chemical content composition of the individual grain. The reactivity and solubility level increase with increasing structure modifiers content in particles, so the high silicious S2 ashes contribute lower reactivity compared to calcaneus S1 ashes. Also, for this reason, the S1 sample structure is denser, and more hydration products can be observed. [15,46,57,62] It was also observed a difference in microscale structure formation for S1 and S2 ashes, whereas, for the S1 sample, highly dense needle crystals are abundant. Those needle crystals are an Al-Ca-S-hydrated needle-shaped ettringite mineral crystals, formed in the presence of high concentrations of SO 4 -2 and the presence of elevated CaO content (as in the case of S1 ashes) [63,64]. The formation of ettringite is enhanced by the high containment of Al oxides, available from mineral decompositions and amorphous phase. This contributes to the crystalline phase formation which affects the structure, as pores and free spaces become filled with needles. The ettringite formation can be responsible for the degradation of cementitious materials, through the swelling of the material followed by crack diffusion in the structure[63,65,66]. Gesoğlu et all. [67] show that for porous materials, such as fly ash clay-cement suspensions discussed in this study, ettringite crystal growth does not pose a risk of expansion cracking, because those crystals grow in pores and empty spaces in structure, causing an increase in final strain, structure tightness, and potentially causing an increase in permeability properties [68–70]. So the highly reactive S1 particles start to dissolve and intersect with the surroundings, in a result filling the pores and creating a more dense structure compared to S2. For the S2 samples, mostly cement hydration phases are observed while ash particles remain unreacted. Worth noticing is the influence of agglomerates and “pocket-enclosed” grains in S1.O and S2.O ashes (Fig. 10). These agglomerates cause formations of regions in the structure, where clusters of unreacted ashes are present, providing anisotropy to the structure. The pocket-enclosed grains result in the immobilization of some potentially reactive grains. Those effects cause the final strain to decrease for S1.O and S2.O ash suspensions. For other fractions, those effects have less impact because performed aerodynamic separation processes cause a disintegration effect, where low-durable grains and agglomerates undergo breakdown and ashes obtain a higher level of dispersion [39,40]. As a result, a higher amount of individual particles can be released and participate in structure formation. Fractionation has a significant impact on structure formation intensity , hydration processes and grain reactivity. 4. Conclusions The separation of fly ash into different size fractions results in fractions with varying chemical, mineralogical, and physical characteristics. Finer fractions contain increased levels of reactive aluminum, calcium, and sulphur compounds compared to coarser with more silica-rich content. Finer ash fractions possess higher reactivity, evidenced by rapid viscosity increases upon water mixing as well as enhanced early strength development. The ultrafine fraction induced flash setting within a few minutes after mixing minutes. In contrast, coarse fractions showed more gradual reactivity behavior over longer timescales. Interactions between the ashes and clay suspensions led to complex rheological impacts dependent on particle fineness, shape, and mineralogy. High calcium S1 ashes resulted in more intense early hydration reactions compared to siliceous S2 ashes. Microstructural analysis correlated the improved compressive strength of clay-cement mortars to the ability of fine ash fractions to accelerate the formation of denser, more uniform structures. The results of this work demonstrate the differences between individual fly ash fractions and their potential to engineer properties of suspension-based construction materials and systems. Declarations Author Contributions: JD contributed to conceptualization, methodology, validation, formal analysis, investigation, data curation, writing—original draft, and visualization. PI and ŁW, contributed to methodology, validation, formal analysis, investigation, data curation, resources, writing—review and editing, and supervision, AS – writing, editing and supervision, MJ – formal analysis Funding: This research received no external funding. Institutional Review Board Statement: Not applicable. Informed Consent Statement: Not applicable. Conflicts of Interest: The authors declare no conflicts of interest. Data Availability Statement: The datasets used and/or analyzed during the current study available from the corresponding author on reasonable request References Alterary, S.S.; Marei, N.H. Fly Ash Properties, Characterization, and Applications: A Review. J King Saud Univ Sci 2021 , 33 , 101536, doi:10.1016/j.jksus.2021.101536. Smoot, L.D.; .Smith, P.J. Coal Combustion and Gasification ; 2010; Kumar, S.; Singh, J.; Mohapatra, S.K. Role of Particle Size in Assessment of Physico-Chemical Properties and Trace Elements of Indian Fly Ash. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-4100023","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":289172002,"identity":"ab7fa6ef-db7c-4a51-b057-03e242898437","order_by":0,"name":"Jurij Delihowski","email":"","orcid":"","institution":"AGH University of Krakow","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Jurij","middleName":"","lastName":"Delihowski","suffix":""},{"id":289172003,"identity":"7941d824-23c4-4733-b448-fb620b2e836f","order_by":1,"name":"Piotr Izak","email":"","orcid":"","institution":"AGH University of Krakow","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Piotr","middleName":"","lastName":"Izak","suffix":""},{"id":289172004,"identity":"190a89b4-4ff0-4c51-a682-ff1b5d3f7de6","order_by":2,"name":"Łukasz Wójcik","email":"","orcid":"","institution":"AGH University of Krakow","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Łukasz","middleName":"","lastName":"Wójcik","suffix":""},{"id":289172005,"identity":"a0089fc8-1f9d-4838-accf-313f1aa239a8","order_by":3,"name":"Agata Stempkowska","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAxklEQVRIiWNgGAWjYNCCCgYGAyAlAcQyhFWzgYgzCC08xGlhbCNFi/z85qObC+fZ2W1nYD54m4fhDmEtBsfY0m7P3JacvLOBLdmah+EZEVrYeMxu825jTjY4wGMmzcNwmAiHtfF/u807px6ohf8bcVoYjvGw3eZtOGwHtIWNOC0Gx9LMbs84djzB4DCbseUcAyL8It98+Nntgppqe4PjzQ9vvKm4I0fYYUDADMSJDcxgSw8QpQOsxR7KJlLLKBgFo2AUjCgAAHYhN8IKKCOsAAAAAElFTkSuQmCC","orcid":"","institution":"AGH University of Krakow","correspondingAuthor":true,"submittingAuthor":false,"prefix":"","firstName":"Agata","middleName":"","lastName":"Stempkowska","suffix":""},{"id":289172006,"identity":"11bbd503-7dba-4714-85d6-3979dd7488d2","order_by":4,"name":"Marcin Jarosz","email":"","orcid":"","institution":"Comex Polska sp. z o.o","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Marcin","middleName":"","lastName":"Jarosz","suffix":""}],"badges":[],"createdAt":"2024-03-14 10:57:17","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-4100023/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-4100023/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1038/s41598-024-72315-0","type":"published","date":"2024-09-14T15:57:10+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":54585305,"identity":"a5f50b97-d170-48a0-a6a9-2694a1f1a014","added_by":"auto","created_at":"2024-04-12 15:37:55","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":238144,"visible":true,"origin":"","legend":"\u003cp\u003eGranulometric distribution of obtained fly ash fractions: (a) S1 ashes; (b) S2 ashes.\u003c/p\u003e","description":"","filename":"1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/f6976f21d32aa7541d8af713.jpg"},{"id":54585303,"identity":"bb481178-e458-4a92-b015-b829ba6e51a5","added_by":"auto","created_at":"2024-04-12 15:37:54","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":104276,"visible":true,"origin":"","legend":"\u003cp\u003eDensity and surface area of obtained ash fractions\u003c/p\u003e","description":"","filename":"2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/507488f2895d0a2ddca77d7f.jpg"},{"id":54586028,"identity":"91e3544b-6572-4e25-b372-ecd09cf37b89","added_by":"auto","created_at":"2024-04-12 15:45:55","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":156847,"visible":true,"origin":"","legend":"\u003cp\u003eThe influence of ash fraction on the viscosity of water-ash suspensions viscosity; fly ash short-time reactivity. Water/ash (w/a) ratio: (a) S1- 10/3; (b) S2 - 1/1.\u003c/p\u003e","description":"","filename":"3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/897fd523c937206bcc8a10f0.jpg"},{"id":54586027,"identity":"b8a720b2-8d0e-41c0-a3a8-49b4f14893f1","added_by":"auto","created_at":"2024-04-12 15:45:55","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":113815,"visible":true,"origin":"","legend":"\u003cp\u003eChange of viscosity in the function of shear rate for S1.O, S1.UF and S2.O, S2.UF fractions. Base clay suspension density 1.20g/cm\u003csup\u003e3\u003c/sup\u003e, cement 10%, fly ash 20%\u003c/p\u003e","description":"","filename":"4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/416185c28a75bfdc4bbdd198.jpg"},{"id":54586026,"identity":"e6fc4401-7162-4a5d-9b60-e1bc02031f12","added_by":"auto","created_at":"2024-04-12 15:45:55","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":222915,"visible":true,"origin":"","legend":"\u003cp\u003eThe influence of fly ash fraction on the suspension viscosity: S1 20%, cement 10%, density 1.13g/cm\u003csup\u003e3\u003c/sup\u003e; S2 20%, cement 10%, density 1.20g/cm\u003csup\u003e3\u003c/sup\u003e\u003c/p\u003e","description":"","filename":"5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/d3af65f2e5ae2352270d37b9.jpg"},{"id":54585311,"identity":"c57da941-903b-49aa-9490-735371b89f0f","added_by":"auto","created_at":"2024-04-12 15:37:55","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":218135,"visible":true,"origin":"","legend":"\u003cp\u003eCompressive strain for samples with S1 ash fractions: cement 10%wt, base suspension density 1.13g/cm\u003csup\u003e3\u003c/sup\u003e; With S2 ahs fractions: cement 10%, base suspension density 1.20g/cm\u003csup\u003e3\u003c/sup\u003e.\u003c/p\u003e","description":"","filename":"6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/bc0a73b46fe5f94ad058b0ff.jpg"},{"id":54585310,"identity":"74e431d8-277c-45ec-9f92-194580c25f79","added_by":"auto","created_at":"2024-04-12 15:37:55","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":578228,"visible":true,"origin":"","legend":"\u003cp\u003eMicrostructure evolution SEM images. S1.O (a, b, c) and S2.O (d, e, f) at 7, 28, and 90 days of curing. Fly ash 20%, cem.10%, 1.13 and 1.20 g/cm\u003csup\u003e3\u003c/sup\u003e respectively.\u003c/p\u003e","description":"","filename":"7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/b2d7230866576a0cf2387215.jpg"},{"id":54586029,"identity":"4b57a609-e514-4e2d-8cd8-fb8ddafc9db4","added_by":"auto","created_at":"2024-04-12 15:45:56","extension":"jpg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":307017,"visible":true,"origin":"","legend":"\u003cp\u003eMicrostructure differences depending on grain type: a) coarse C grains, b) middle M grains; c) fine UF grains evolution SEM images.\u003c/p\u003e","description":"","filename":"8.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/37a29f53fd5771ddcc0fc1b1.jpg"},{"id":54585309,"identity":"068165c2-2866-49f9-a732-426e37e53c1d","added_by":"auto","created_at":"2024-04-12 15:37:55","extension":"jpg","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":258309,"visible":true,"origin":"","legend":"\u003cp\u003eGrain reactivity in the function of chemical composition at 90 day with point EDS analysis: a) high Al-Si grain; b) medium Al-Si grain; c) high Ca grain.\u003c/p\u003e","description":"","filename":"9.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/95ef56a42eb08af71b72d42b.jpg"},{"id":54585308,"identity":"fae30d19-d23c-4f9e-9557-0a5dfcb15415","added_by":"auto","created_at":"2024-04-12 15:37:55","extension":"jpg","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":191022,"visible":true,"origin":"","legend":"\u003cp\u003ea) Cluster of fine grains inside a larger grain, sample S2.O at 90 day of curing; b) Immobilized grains in \"pockets\".\u003c/p\u003e","description":"","filename":"10.jpg","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/5ddaa73115a83eefd622e09a.jpg"},{"id":64619328,"identity":"b7374f20-b5b2-480f-808c-4ccbde1939d9","added_by":"auto","created_at":"2024-09-16 16:14:08","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":3190610,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4100023/v1/8ee7311c-7597-4c62-a705-1f7aa0318700.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"The influence of selected grain size fractions of coal fly ash on properties of clay-cement mortars used for the flood levees construction","fulltext":[{"header":"HIGHLIGHTS","content":"\u003cp\u003e- The grain fractions of ash affect the rheological properties and mechanical strength of barriers that are used in flood control applications.\u003c/p\u003e\n\u003cp\u003e- Fractionation has a significant impact on structure formation intensity , hydration processes and grain reactivity.\u003c/p\u003e\n\u003cp\u003e-The increase in viscosity immediately after mixing and its effect on the workability of fly ash mixtures for barriers depends primarily on the development of the surface, that is, directly on the size of the particles\u003c/p\u003e"},{"header":"1. Introduction","content":"\u003cp\u003eCoal combustion for energy purposes generates combustion by-products, where fly ash constitutes up to 70-90% of the total by-products \u0026nbsp;[1,2]. Fly ash consists of incompletely burned organic residues and thermally transformed mineral matter present in feedcoal. Pounds and disposals, where those ashes are stored, occupy large natural territories and can have a harmful impact on surrounding areas, underground water, and the atmosphere [3\u0026ndash;6]. Globally, fly ash utilization rates vary: India used 66% of its 233 million tons in 2021 [7], China applied most of its 550 million tons produced in 2018 to construction and cement [8], Australia utilized 47% of 14 million tons in 2019 [9], and Europe used a significant portion of over 1 billion tons produced from 1965 to 2015 in cement and road construction [10]. While some countries achieve 100% utilization, the average global rate is around 60% [11]. Due to the necessity of utilizing incredible amounts of those by-products, numerous applications across various industrial sectors have incorporated fly ashes into production processes. Some examples include its use in ceramics, composite engineering, the cement industry, and soil modification and stabilization additives [4,6,12,13].\u003c/p\u003e\n\u003cp\u003eMineralogical and chemical characteristics of fly ash can vary significantly depending on such factors as coal type and origin, combustion process, and precipitation techniques [2,3,14]. A better understanding of tendencies and variations in fly ash properties can help to design efficient utilization strategies and incorporate ashes in new industries.\u003c/p\u003e\n\u003cp\u003eFly ash processing and separation are commonly used for enhancing ash properties and extracting various grain fractions with desired parameters [3,4]. Concerning this study, the separation due to the grain size will be briefly discussed. In general, fine-grained fractions are associated with increased levels of certain phases, e.g. alumo- and calcium-silicates. These phases are known to be important for the pozzolanic properties of fly ash, which enhance the strength and durability of concrete [15\u0026ndash;17]. In terms of chemical composition, those fine ash fractions tend to be enriched in certain oxides, e.g. sulphur, chlorine, and potassium as well as some trace elements, e.g. Mn, Mg, Zn, Cr, Ni and Pb [4].\u003c/p\u003e\n\u003cp\u003eMiddle-sized and coarse fractions generally have different mineralogical and chemical characteristics compared to fine fractions [3,15]. Coarse fractions tend to be enriched in crystalline phases, including significant levels of mullite and quartz as well as unburned feedcoal grains. These mineral grains can act as supplementary inert unreactive fillers in constructions and concrete. By subjecting coarse fractions to additional pretreatment (mechanical, chemical, or thermal), their reactive potential can be activated, which in turn, transforms them into active pozzolanic additives [18\u0026ndash;21].\u003c/p\u003e\n\u003cp\u003eMiddle-sized fractions are also known to have some pozzolanic properties [22,23]. The chemical composition of middle-sized fractions generally contains lower levels of active elements compared to fine fractions and a higher amount of amorphous fractions compared to a coarse fraction. Worth, noticing is a high level of porosity and the highest level of presence of cenospheres in this fraction [24\u0026ndash;26]. This can make them a more attractive option for certain specific applications where some restrictions to building materials are required, e.g. lightweight building materials, thermal insulators, etc [6,12,13].\u003c/p\u003e\n\u003cp\u003eAmong many other applications, fly ash has become a popular filler material for hydraulic structures and, in particular, clay-cement suspensions for flood-levees construction [27,28]. Those sealing suspensions consist of base clay-water suspension and cement, forming a thixotropic fluid that can be pumped and introduced into embankments, gaining strength over time. They provide the necessary strength, stability, and water resistance for levees. In these suspensions, clay provides cohesive and impermeable properties, while the cement acts as a binder that improves strength in the later stages of curing. The interactions between the clay platelets, cement hydration products and water create a complex microstructure resembling a continuous 3D network with mechanical durability and infiltration properties [29\u0026ndash;31].\u003c/p\u003e\n\u003cp\u003eFly ash additives can influence this network in several ways. The reactions between clay minerals, cement and fly ash modifies the fresh mortars rheology and further microstructural development during the curing stages. The fly ash particles are capable of filling voids, enhancing packing density, and increasing infiltration properties. Moreover, the increased surface area of ashes offers additional sites for hydration and pozzolanic reactions. In addition, fly ash additives can improve chemical resistance and as a result, increase the durability and safety of structures [28,30\u0026ndash;32].\u003c/p\u003e\n\u003cp\u003eIn this study, the influence of selected fly ash fractions on the properties of clay-cement sealing suspensions used for flood levees was investigated. The influence of the addition of different grain size fractions on rheological properties and compressive strength was examined and discussed. The results can contribute to a better understanding of the possibilities of using selected ash fractions and their impact on the properties of final products.\u003c/p\u003e"},{"header":"2. Materials and methods","content":"\u003cp\u003e2.1 Materials\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eFly ash\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eTwo different types of fly ashes from Polish power plants were used:\u003c/p\u003e\n\u003cp\u003eS1 \u0026ndash; High calcareous fly ash from lignite combustion (S1.O), obtained from Belchat\u0026oacute;w power plant, Poland, from the combustion of brown coal.\u003c/p\u003e\n\u003cp\u003eS2 \u0026ndash; Silicious fly ash from bituminous coal (S2.O), from Krak\u0026oacute;w power plant, Poland.\u003c/p\u003e\n\u003cp\u003eGranulometric separation was used to obtain representative fractions. The chemical, mineralogical, and granulometric composition of obtained fractions is presented in the following parts.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eCement\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe Cement CEM I 42.5 R Odra Opole, produced by Cement plant \u0026quot;Odra\u0026quot; S.A., is composed of Portland clinker in the range of 95-100% and secondary components such as gypsum in the range of 0-5%. The chemical composition is presented in Table 1.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eTable 1.\u003c/strong\u003e Chemical composition of Cement CEM I 42,5 R Odra Opole\u003c/p\u003e\n\u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd width=\"100%\" colspan=\"6\" valign=\"top\"\u003e\n \u003cp\u003eChemical composition (%wt.)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eAl\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eFe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eCaO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eMgO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003eNa\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003eeq\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e19.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e6.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e2.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e63\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e1.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"16.666666666666668%\"\u003e\n \u003cp\u003e0.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003e\u003cem\u003eClay\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe mineral accompanying the brown coal deposits in the Bełchat\u0026oacute;w mine was used as the clay raw material. The Bełchat\u0026oacute;w clay present in this paper is the most common clayey silt in this deposit. Chemical composition is presented at Table 2.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eTable 2.\u003c/strong\u003e Chemical composition of Clay Bełchat\u0026oacute;w\u003c/p\u003e\n \u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\" width=\"521\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd width=\"100%\" colspan=\"11\"\u003e\n \u003cp\u003eChemical composition (%wt.)\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd width=\"8.637236084452976%\"\u003e\n \u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"10.556621880998081%\"\u003e\n \u003cp\u003eAl\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.061420345489443%\"\u003e\n \u003cp\u003eCaO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.829174664107486%\"\u003e\n \u003cp\u003eMgO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"10.36468330134357%\"\u003e\n \u003cp\u003eFe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.829174664107486%\"\u003e\n \u003cp\u003eMnO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"11.324376199616124%\"\u003e\n \u003cp\u003eNa\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.061420345489443%\"\u003e\n \u003cp\u003eK\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.445297504798464%\"\u003e\n \u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"9.404990403071018%\"\u003e\n \u003cp\u003eH\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"7.485604606525912%\"\u003e\n \u003cp\u003eLOI\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd width=\"8.637236084452976%\"\u003e\n \u003cp\u003e58.65\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"10.556621880998081%\"\u003e\n \u003cp\u003e14.55\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.061420345489443%\"\u003e\n \u003cp\u003e4.75\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.829174664107486%\"\u003e\n \u003cp\u003e0.72\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"10.36468330134357%\"\u003e\n \u003cp\u003e3.46\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.829174664107486%\"\u003e\n \u003cp\u003e0.72\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"11.324376199616124%\"\u003e\n \u003cp\u003e1.02\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.061420345489443%\"\u003e\n \u003cp\u003e1.05\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"8.445297504798464%\"\u003e\n \u003cp\u003e0.42\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"9.404990403071018%\"\u003e\n \u003cp\u003e5.52\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd width=\"7.485604606525912%\"\u003e\n \u003cp\u003e9.72\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003eFrom a mineralogical point of view, this clay consists mainly of beidellite and quartz\u003c/p\u003e\n\u003cp\u003e2.2. Methods\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eChemical composition analysis XRF\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe WD-XRF spectrometer S8 TIGER from Bruker was used for the analysis. The measurements were performed using the vacuum method with the built-in Quant Express reference standard.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eMineralogical analysis XRD\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe phase composition of the ashes was determined using a PANalytical Empyrean X-ray diffractometer. The measurements were performed using monochromatic radiation with a wavelength corresponding to the copper K(\u0026alpha;1) emission line (1.54178 \u0026Aring;), in the angular range of 5-90 degrees in 2\u0026theta; scale, with a goniometer step size of 0.008 degrees. The qualitative analysis of the phase composition was carried out using the X\u0026apos;Pert HighScore Plus computer program developed by PANalytical. The reference databases: PDF-2 (2004) and ICSD Database FIZ Karlsruhe (2012).\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eLost of ignitions (LOI)\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eLOI tests were performed according to the ASTM D7348 procedure. In the first step, the sample was weighted and heated at 110\u0026nbsp;̊C for 1 hour. Then, the sample was placed in a desiccator to cool for 60 min before being reweighted. The weight loss in this step was recorded as moisture content. In the second step, dried fly ash was placed in a furnace and heated in a stepped schedule for 2 hr to reach 950\u0026nbsp;̊C. The fired sample was cooled down to room temperature in a desiccator and then weighted. The weight loss associated with firing the sample is known as the loss of ignition (LOI).\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eDensity analysis\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eDensity analysis was performed using the volumetric method in a discontinuous manner with the Micromeritics ASAP 2010. The sample was degassed at 350C for 24 hours under a vacuum of 10-3 mmHg. The BET multi-point method was used to determine the specific surface area at relative pressures ranging from 0.05 to 0.30. Volume calibration was performed by the apparatus before the actual measurement. Nitrogen with a purity of 99.999% was used as the adsorbate, and the measurement was conducted at the temperature of liquid nitrogen.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eRheological measurements\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eFor the rheological studies, a Brookfield DV-III+ rheometer with a coaxial cylinder system was used, which allows for the measurement of shear stress or viscosity of liquids at different shear rates.\u003c/p\u003e\n\u003cp\u003eThe first part of the rheological investigation focused on studying the short-time reactivity of fly ashes, both S1 and S2, and their fractions. The tests were performed using water-fly ash suspensions, where the ash-to-water ratio was adjusted (w/a). For S1 fly ashes, w/a ratio was set at 10/3, and for S2 fly ashes at 1/1. These ratios were chosen based on noticeable differences in water demand and the suspensions\u0026apos; workability, with S1 ashes exhibiting greater reactivity compared to S2 ashes. The measurement was performed at a constant shear rate of 20 rpm immediately after suspension preparation. The test duration time was 40 minutes. Obtained changes in suspension viscosity provided insights into the short-time reactivity of the fly ashes, concerning their ability to react with water immediately after mixing and their ability to form a spatial structure. Results of the short-time reactivity of fly ashes are presented in Figure 3.\u003c/p\u003e\n\u003cp\u003eThe second part of the rheological tests involved measuring the rheological properties of various fly ash\u0026ndash;clay-cement mixtures. The viscosity measurements were conducted using an algorithm where the shear rate was incremented by 2.0 rpm every 30 seconds. The rheometer started at 2.0 rpm and the data at each speed change was collected, up to a maximum of 40.0 rpm. Then, a second stage of measurements takes place, and the shear rate decreases until reaching 2.0 rpm. For each data point the apparent viscosity, shear stress, and time were measured.\u003c/p\u003e\n\u003cp\u003eMixtures were prepared for the 20%, 30% and 40% fly ash additives by weight. Where for S1 ashes the base suspension density of 1.13 g/cm\u003csup\u003e3\u003c/sup\u003e was selected, and for S2 ashes 1.20g/cm\u003csup\u003e3\u003c/sup\u003e. Cement in all mixtures states 10% by weight. Such recipes allow for the most appropriate measurement.\u003c/p\u003e\n\u003cp\u003eResults for the rheological properties of various fly ash-clay-cement mixtures are presented in Figure 4 and Figure 5.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eMechanical measurements\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe compressive strain tests were conducted using the ZwickRoell Tira Test 2300 mechanical testing machine with Senga software. Cylindrical samples measured 45x45mm were subjected to a curing process submerged in water and were tested after 14, 28, and 90 days of curing.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eSEM and microstructure\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eScanning Electron Microscopy (SEM): Measurements were performed on the obtained fly ash fractions and hardened mortars after 14, 28, and 90 days of curing. The Thermoscientific Fisher Phenom XL SEM equipped with an Energy Dispersive Spectroscopy (EDS) attachment was used. The EDS attachment allows for the efficient determination of the point chemical composition of the tested samples\u003c/p\u003e"},{"header":"3. Results \u0026 Discussion","content":"\u003cp\u003e3.1. Fly ash fractions characteristic\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eGranulometry and microstructure characteristic\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe dry aerodynamic separation process resulted in the obtaining of different fractions based on the grain size distribution. The ACX separator produced by COMEX Polska sp.zoo. was used [33]. These fractions include:\u003c/p\u003e\n\u003cul class=\"decimal_type\"\u003e\n\u003cli\u003e\n\u003cp\u003eUltra Fine fraction (UF): particles with a grain size range of 0 to 10 \u0026mu;m. It consists of the finest obtained particles.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eFine fraction (F) has a grain size distribution from around 5 to 20 \u0026mu;m. This fraction contains particles slightly larger than those in the UF fraction.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eMiddle fraction (M) was obtained through manual sieving of the residues from aerodynamic separation by using a 100 \u0026mu;m mesh sieve, resulting in grain size range from approx. 20 to 100 \u0026mu;m, and represents particles of intermediate range size.\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eCoarse fraction (C) mainly consists of grains larger than 100 \u0026mu;m and represents the residues on top of the 100 \u0026mu;m sieve.\u003c/p\u003e\n\u003c/li\u003e\n\u003c/ul\u003e\n\u003cp\u003eThe d\u003csub\u003e90\u003c/sub\u003e, d\u003csub\u003e50\u003c/sub\u003e and d\u003csub\u003e10\u003c/sub\u003e parameters in Table 3. were used to determine fractions size, representing percentiles denoted by the letter d followed by the % value. Thus, d\u003csub\u003e10\u003c/sub\u003e = 1.7\u0026micro;m means that 10% of the particles are smaller than 1.7\u0026micro;m, etc. Figure 1 presents the granulometric distribution of obtained fractions as a cumulative volume chart.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eTable 3.\u003c/strong\u003e Fly ash fractions granulometry\u003c/p\u003e\n\u003ctable border=\"1\" width=\"528\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"7.9245283018867925%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"6.7924528301886795%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003eS1.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.679245283018869%\"\u003e\n\u003cp\u003eS1.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003eS1.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.3584905660377355%\"\u003e\n\u003cp\u003eS1.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.433962264150944%\"\u003e\n\u003cp\u003eS1.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003eS2.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.056603773584905%\"\u003e\n\u003cp\u003eS2.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003eS2.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.3584905660377355%\"\u003e\n\u003cp\u003eS2.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.433962264150944%\"\u003e\n\u003cp\u003eS2.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd rowspan=\"3\" valign=\"top\" width=\"7.9245283018867925%\"\u003e\n\u003cp\u003eDistribution (\u0026mu;m)\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"6.7924528301886795%\"\u003e\n\u003cp\u003ed\u003csub\u003e10\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003e1.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.679245283018869%\"\u003e\n\u003cp\u003e69.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003e22.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.3584905660377355%\"\u003e\n\u003cp\u003e1.17\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.433962264150944%\"\u003e\n\u003cp\u003e0.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003e3.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.056603773584905%\"\u003e\n\u003cp\u003e73.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"8.49056603773585%\"\u003e\n\u003cp\u003e17.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.3584905660377355%\"\u003e\n\u003cp\u003e1.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.433962264150944%\"\u003e\n\u003cp\u003e0.4\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"7.377049180327869%\"\u003e\n\u003cp\u003ed\u003csub\u003e50\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e28.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.426229508196721%\"\u003e\n\u003cp\u003e159.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e53.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.991803278688525%\"\u003e\n\u003cp\u003e7.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"10.245901639344263%\"\u003e\n\u003cp\u003e2.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e21.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.836065573770492%\"\u003e\n\u003cp\u003e179.2\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e52.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.991803278688525%\"\u003e\n\u003cp\u003e5.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"10.245901639344263%\"\u003e\n\u003cp\u003e2.4\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"7.377049180327869%\"\u003e\n\u003cp\u003ed\u003csub\u003e90\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e140.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.426229508196721%\"\u003e\n\u003cp\u003e349.8\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e101.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.991803278688525%\"\u003e\n\u003cp\u003e19.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"10.245901639344263%\"\u003e\n\u003cp\u003e9.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e142.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.836065573770492%\"\u003e\n\u003cp\u003e338\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"9.221311475409836%\"\u003e\n\u003cp\u003e102.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"7.991803278688525%\"\u003e\n\u003cp\u003e21.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"10.245901639344263%\"\u003e\n\u003cp\u003e10.5\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003e\u003cem\u003eChemical and mineralogical composition\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe chemical composition of obtained fractions for S1 and S2 ashes is presented in Table 4.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eTable 4.\u0026nbsp;\u003c/strong\u003eChemical composition of S1 and S2 fly ash fractions\u003c/p\u003e\n\u003ctable border=\"1\" width=\"697\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd colspan=\"12\" width=\"100%\"\u003e\n\u003cp\u003eChemical composition (% wt)\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003eS1.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003eS1.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003eS1.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003eS1.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003eS1.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003eS2.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003eS2.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003eS2.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003eS2.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003eS2.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eSiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e30.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e44.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e28.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e21.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e16.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e54.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e58.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e51.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e49.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e48.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eAl\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e30.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e33.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e28.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e26.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e24.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e24.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e23.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e23.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e29.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e30.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eCaO\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e24.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e12.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e25.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e33.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e37.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e5.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e3.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e6.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e4.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e4.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eSO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e2.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e3.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e4.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e6.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e0.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e1.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e1.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eFe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e9.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e5.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e10.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e10.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e10.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e8.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e7.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e9.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e6.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e5.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eMgO\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e1.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e1.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e1.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e1.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e3.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e2.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e4.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e2.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e2.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eTiO\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e0.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e1.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e1.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e1.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eP\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e0.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e0.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e0.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e0.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eK\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e0.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e0.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e2.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e2.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e2.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e3.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e3.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eNa\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e1.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e0.6\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e1.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e2.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e2.4\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eTotal\u0026nbsp;Ʃ\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"6.618705035971223%\"\u003e\n\u003cp\u003e98.0\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"8.201438848920864%\"\u003e\n\u003cp\u003e100.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"9.06474820143885%\"\u003e\n\u003cp\u003e99.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"7.76978417266187%\"\u003e\n\u003cp\u003e98.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"10.647482014388489%\"\u003e\n\u003cp\u003e97.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"8.489208633093526%\"\u003e\n\u003cp\u003e100.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"8.201438848920864%\"\u003e\n\u003cp\u003e99.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"9.06474820143885%\"\u003e\n\u003cp\u003e99.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"7.76978417266187%\"\u003e\n\u003cp\u003e101.1\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"bottom\" width=\"10.647482014388489%\"\u003e\n\u003cp\u003e99.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"13.381294964028777%\"\u003e\n\u003cp\u003eLOI\u003cbr /\u003e\u0026nbsp;(% of total mass)\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"6.618705035971223%\"\u003e\n\u003cp\u003e1.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e6.5\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e0.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e1.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e1.8\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.489208633093526%\"\u003e\n\u003cp\u003e11.2\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"8.201438848920864%\"\u003e\n\u003cp\u003e14.9\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"9.06474820143885%\"\u003e\n\u003cp\u003e7.7\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"7.76978417266187%\"\u003e\n\u003cp\u003e13.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"10.647482014388489%\"\u003e\n\u003cp\u003e13.3\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"0.14388489208633093%\"\u003e\n\u003cp\u003e\u0026nbsp;\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003eThe mineralogical composition is presented in Tables 5 and Table 6. The identified phases in each fraction are denoted using a ranking scale to indicate the relative abundance:\u003c/p\u003e\n\u003cp\u003e\"-\" indicates the absence or very low phase presence;\u003c/p\u003e\n\u003cp\u003e\"+\" denotes a minor amount of the phase;\u003c/p\u003e\n\u003cp\u003e\"++\" signifies the phase presence in moderate quantities;\u003c/p\u003e\n\u003cp\u003e\"+++\" represents a high amount of the phase compared to other fractions.\u003c/p\u003e\n\u003cp\u003eIn Figure 2 density and obtained surface area of fractions are presented.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eTable 5.\u003c/strong\u003e Mineralogical composition of S1 ash fractions\u003c/p\u003e\n\u003ctable border=\"1\" width=\"530\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eIdentified phase\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003eS1.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003eS1.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003eS1.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003eS1.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003eS1.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eCalcite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e\u0026nbsp;-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eEckermannite-\u003cbr /\u003e\u0026nbsp;gehlenite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eQuarts low\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eAnhydrite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eHematite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eMullite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eLime\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eComplex\u0026nbsp;\u003cbr /\u003e\u0026nbsp;high-calcium oxides\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd valign=\"top\" width=\"26.037735849056602%\"\u003e\n\u003cp\u003eAmorphous\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.339622641509434%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd valign=\"top\" width=\"16.41509433962264%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003e\u003cstrong\u003eTable 6.\u003c/strong\u003e Mineralogical composition of S2 ash fractions\u003c/p\u003e\n\u003ctable border=\"1\" width=\"530\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n\u003ctbody\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eIdentified phase\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003eS2.O\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003eS2.C\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003eS2.M\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003eS2.F\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003eS2.UF\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eCalcite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e\u0026nbsp;-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eMullite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eQuartz low\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eHematite\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eLime\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e+\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e-\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003ctr\u003e\n\u003ctd width=\"26.037735849056602%\"\u003e\n\u003cp\u003eAmorphous\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.339622641509434%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.90566037735849%\"\u003e\n\u003cp\u003e++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"14.150943396226415%\"\u003e\n\u003cp\u003e+++\u003c/p\u003e\n\u003c/td\u003e\n\u003ctd width=\"16.41509433962264%\"\u003e\n\u003cp\u003e+++\u003c/p\u003e\n\u003c/td\u003e\n\u003c/tr\u003e\n\u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003eThe X-ray diffraction analysis of S1 fly ash samples highlights a variety of complex high-calcium oxides with increasing concentrations in finer fractions S1.F and S1.UF. Those are calcium sodium aluminum oxide, calcium aluminum oxide sulfate, calcium iron aluminum oxide, and calcium magnesium aluminum silicate. These oxides are characterized by structurally modified forms with variable chemical compositions, which also affects their reactivity. Compounds involving calcium, aluminum, and sulfate ions can participate in various chemical reactions when exposed to water. For instance, calcium sodium aluminum oxide might form aluminum hydroxide and sodium hydroxide, releasing heat in the process when exposed to water. Calcium aluminum oxide sulfate is the anhydrite/gypsum-like phase that can undergo relatively rapid surface hydration reactions with water, increasing viscosity. The presence of these minerals in finer fractions suggests quicker hydration reactions due to larger surface areas and fineness of grains [34\u0026ndash;38].\u003c/p\u003e\n\u003cp\u003eWorth noticing, that the mineral distribution across grain sizes in fly ashes indicates a \"disintegration effect\"[39,40]. Hard minerals like quartz, show a lower tendency to be affected by mechanical separation, typically remaining in the coarser fractions. Conversely, softer minerals like anhydrite appear more frequently in the finer fractions, due to their greater susceptibility to breakdown during processing. Such low-durable minerals concentrated in fine fractions strongly influence short-time reactivity thus causing viscosity increase. Gehlenite, a mineral containing calcium and silica, can react with water and contribute to a rapid viscosity increase in the suspension. Anhydrite can interact with water to form gypsum and the potential formation of ettringite from calcium aluminum oxide sulfate. The S1 fly ashes contain an increased amount of these and other compounds, which are unevenly distributed throughout the particle size range, contributing to the difference in reactivity among the fractions (Tab.4) [41\u0026ndash;45].\u003c/p\u003e\n\u003cp\u003eThe observed mineralogical distribution finds a response in the chemical composition results of fly ash samples S1 and S2, with a focus on their finer fractions, suggesting that the alumosilicate glass present is likely to exhibit higher levels of modification compared to the coarser fractions [38,46]. In finer fractions, the glass phase is expected to be less siliceous and more modified, potentially enriched with network modifiers like calcium, magnesium, sodium, and potassium, as in accordance with the results of the chemical composition analysis. These modifiers disrupt the glass structure, making it more reactive. This contrasts with the coarser fractions, where the glass is anticipated to be more siliceous and less modified, thus more stable and slower in participating in pozzolanic reactions. The composition of the glass phase, including the balance of network formers and modifiers, plays a critical role in the reactivity of the fly ash, influencing the dissolution rates and the formation of strength-enhancing products within the cement matrix.\u003c/p\u003e\n\u003cp\u003e3.2. Rheological Tests\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eShort-time reactivity\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eFor both ashes in water suspensions (Fig.3), the viscosity increase with a measure of time was observed. This suggests that some ash-water reactions start immediately after mixing. The S1 ashes, with their higher calcium content, demonstrate faster reactivity, while the more siliceous nature of S2 results in slower reactivity.\u003c/p\u003e\n\u003cp\u003eNotably, the coarse S1.C fraction, despite having less reactive mineral composition than the S1.UF and S1.F groups show a tendency for quicker viscosity development in the initial stage (2-3 minutes). This behavior can be attributed to the presence of large angular particles which results in interlocking and/or rapid sedimentation of the coarse grains, resulting in a shear-thinning behavior similar to that of sand [47].\u003c/p\u003e\n\u003cp\u003eHowever, it is observed that the viscosity increases in fine S1.F and S1.UF fractions are lower compared to S1.M fraction (Fig.3(a)). This can be explained by the dominant factor influencing the viscosity increase immediately after mixing for these ashes being the surface area development and thus free water absorption. The S1.M fraction has the highest surface development compared to the other fractions, stating 67 m\u003csup\u003e2\u003c/sup\u003e/g, resulting in the absorption of free water and an accompanying viscosity increase, while for S1.UF and S1.F states 13.1 m\u003csup\u003e2\u003c/sup\u003e/g and 8.2 m\u003csup\u003e2\u003c/sup\u003e/g (Fig.2).\u003c/p\u003e\n\u003cp\u003eFor all S1 samples, the system stabilizes within 15 to 30 min after mixing ensuring the stability of the rheological measurements at a constant level. Stabilization refers to the equilibrium of the phenomena of structure formation and shear-thinning structure destruction.\u003c/p\u003e\n\u003cp\u003eFor S2 ash fractions, the highest viscosity increase rate is observed for S2.C coarse fraction. Similarly to S1.C fraction, this can be related to sedimentation and interlocking effects of coarse angular grains. Medium S2.M fraction shows very similar characteristics to the original S2.O ash with a slight viscosity increase after the 25th minute of measurement which can suggest at the starting of hydration reactions\u0026mdash;the ultrafine S2.UF fraction does not show reactivity ability as it was in S1.F and S1.UF fine fractions. Furthermore, the high spherical S2.F and S2.UF ashes cause a decrease in suspension viscosity compared to the original ash S2.O, probably due to the ball-bearing effect [48\u0026ndash;50]. Generally, due to the relatively high Si-Al composition and low Ca-compounds of S2 bituminous ashes, a low level of short-time reactivity is observed.\u003c/p\u003e\n\u003cp\u003eIn summary, the increase in viscosity immediately after mixing and its impact on the workability of the fly ash mixtures is primarily influenced by surface development and water absorption. Secondary influences have the presence of reactive minerals and compounds, as well as the shape of the individual particles. The presence of spherical grains results in a reduction of internal friction, while coarse angular fractions cause an interlocking thickening effect. However, further analysis would be required to fully understand all the processes influencing the viscosity changes and setting of the water-ash suspensions.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eSealing suspensions rheology\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe figures in this chapter present a sealing suspension viscosity change as a function of the shear rate. The solid-filled markers present the part of the measurement for increasing shear rate speeds, and no-filled markers \u0026ndash; for the decreasing shear rates. Figure 4 presents the comparison between S1.O, S1.UF and S2.O, S2.UF samples with identical suspension proportions: fly ash 20%, cement 10%, base suspension density 1.20g/cm\u003csup\u003e3\u003c/sup\u003e. Course fractions C, due to the large grains, provide significant distortions to rheological measurement results, making them meaningless and causing a high probability of damaging the equipment. For those reasons, Coarse fraction studies were limited in this work.\u003c/p\u003e\n\u003cp\u003eThe S1 ashes, due to their high reactivity, show a fast viscosity increase. The S1.O sample shows shear thickening characteristics [47,51]. Addition 20% of high reactive S1.UF fraction to the 1.20g/cm\u003csup\u003e3\u003c/sup\u003e dense suspension results in the extension of a measurement scope after the first measuring point. Therefore, in further measurements for S1 ashes samples, to obtain sufficient workability, the base suspension density of 1.13g/cm\u003csup\u003e3\u003c/sup\u003e was used.\u003c/p\u003e\n\u003cp\u003eThe less reactive S2 ashes demonstrate the shear thinning behavior, whereas curves for decreasing share rates lay lower than for increasing share rates. The S2.UF fraction additive shows an increase in viscosity compared to the S2.O fraction, which is inconsistent with the results from the previous section (Fig.3). It can be probably related to clay particles in suspensions which block or reduce the friction-thinning ball-bearing effect of the ash grains. This also indicates that the behavior of fly ash fractions differs when tested in pure water as compared to when tested in a clay-water suspension.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eFly Ash granulometry influence\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eFine fractions S1.F and S1.UF shows the behavior according to expectations and cases of fast viscosity increase after mixing (Fig.5). The reduction of S1 fly ash particle size cases in an increase in the viscosity of clay-cement suspensions. In the high shear rate region, the balance between suspension structure formation and destruction is obtained. At lower shear rates area, an increase in stress can be observed due to faster structure rebuilding, leading to an increase in viscosity. For S1.UF suspension the viscosity acquires values beyond the measurement range at a shear rate of 20 rpm. Similarly, the S1.F fraction results in a constant increase of viscosity followed by an exceeding of scope.\u003c/p\u003e\n\u003cp\u003eIt is worth noting that for the S1.M fraction, based on ash-water reactivity results (Fig.3), the highest viscosity development in clay-cementitious suspension was expected. However, the S1.M viscosity behavior is not consistent with those expectations, and the obtained results remain relatively low in a whole range of measurements. This indicates that the S1.M ash does not possess reactive properties to the same extent as the S1.UF and S1.F fractions and the described viscosity increase in S1.M water suspension (Fig.3) were mainly caused by the absorption of free water in fly ash surfaces. Meanwhile, in the case of clay-based suspensions (Fig.5), a relatively low viscosity level may be attributed to the following factors:\u003c/p\u003e\n\u003cul\u003e\n\u003cli\u003e\n\u003cp\u003eClay particles form a layer on the surface of the fly ash, acting as a surface agent and blocking water molecules' access to the ash surface. This layer can act as a barrier, preventing water from reaching pores, voids, and cracks on the ash surface where it could be adsorbed. This hinders the water absorption process so more free water stays in suspension and viscosity stays relatively low [52];\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eClay particles can form aggregates and structural networks in water-clay suspensions, phenomena related to this ability are well-studied in literature [47,52,53]. These structures can block the movement of water molecules, reducing the availability of adsorption sites on the fly ash surface. This also slows down the water absorption by ash;\u003c/p\u003e\n\u003c/li\u003e\n\u003cli\u003e\n\u003cp\u003eClay particles contribute the ability to water absorption on their surface and by their internal structure. If clay particles are present in a high concentration in a clay-water suspension, they can adsorb water, competing with fly ash. This can reduce the available surface area for water adsorption by fly ash particles, as water molecules are bound to clay minerals so maintaining free water in suspension and enhancing flowability etc.[54\u0026ndash;56]\u003c/p\u003e\n\u003c/li\u003e\n\u003c/ul\u003e\n\u003cp\u003eFor the S2 ashes, the addition of S2.F fraction allows for a viscosity reduction compared to both S2.M and S2.UF fractions. This can be related to the interaction between clay particles and ash grains, where S2.F grains are large enough to cause a ball-bearing effect and reduce suspension internal friction. While for F2.UF ultra-fine grains, the clay particles can cover ash surfaces and block their ball-bearing behavior which causes the suspension viscosity to increase. For coarser F2.M fraction, as was expected according to short-time reactivity results from Figure 3, the suspension viscosity reached the highest values. The addition of obtained fractions case in increasing suspension viscosity compared to S2.O original ashes.\u003c/p\u003e\n\u003cp\u003e3.3. Compressive strain and microstructure analysis results\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eCompressive strain results\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eIn to the base clay-water suspension with a density of 1.13g/cm\u003csup\u003e3\u003c/sup\u003e for S1 ashes and 1.20g/cm\u003csup\u003e3\u003c/sup\u003e for S2 ashes, the 10% of cement and the 20%, 30%, and 40%wt of individual fly ash fractions were added and mixed. Differences in base suspension density are related to the workability of fresh mixtures. The results of comprehensive strain tests at 14, 28, and 90 days of underwater curing are presented in Figure 6.\u003c/p\u003e\n\u003cp\u003eThe obtained results show that decreasing the fineness of fly ash fractions increased obtained compressive strength for both S1 and S2 ashes, resulting at 2.48, 2.65, 2.97, 4.70 and 6.93 MPa for S1.O, S1.C, S1.M, S1.F and S1.UF 40%; and 4.46, 1.71, 4.30, 5.75 and 5.95 MPa for S1.O, S2.C, S2.M, S2.F and S2.UF 40% samples respectively. The 40% ultrafine fraction S1.UF additive gave the maximum obtained strain of tasted recipes showing approx. 179% strain improvement compared to S1.O original ash, while for S2.UF 40% sample this improvement states approx. 33% compared to S2.O.\u003c/p\u003e\n\u003cp\u003eThese strain improvements can be attributed to several factors among which is the chemical and mineralogical composition of fractions with a higher concentration of reactive mineral phases in the finer fractions. In addition, particle fineness promotes more active participation of grains in structure-forming reactions due to the increased contact between the particle surfaces and water, compared to coarser grains. On the other hand, the particle size of F and UF fractions influences suspension workability and structure arrangement. As a result, the denser and more compact microstructure is formed, with individual grains undergoing a more extensive reaction. This reduction in porosity and enhanced interaction contributes significantly to the compressive strain development. Microstructure analysis confirms that coarse grain addition causes the formation of a structure with large pores and cracks, while fine fractions result in a dense uniform structure. Figure 8 shows the influence of particle size on the microstructure formations. For both ashes, there is a noticeable intensification of strain gain at later stages, which is consistent with the theory of delayed reactions in fly ashes [16,23,57].\u003c/p\u003e\n\u003cp\u003eWorth noticing is the variance in base suspension densities used to achieve the optimal workability of mixtures, with S1 ashes having a density of 1.13 g/cm\u0026sup3; and S2 ashes at 1.20 g/cm\u0026sup3;. Due to this difference, direct comparisons of the two ash types at the same replacement levels based on module values of final strain results are not appropriate. However, an analysis of the nature of strength development over time can be performed: S1 ashes showed faster early compressive strain development in the 14-28 day period followed by slower later-stage strain gain compared to S2 ashes. S2 ashes instead had low initial strength gain but higher late-stage strength increased between 28-90 days. This could be attributed to the highly reactive mineralogical compounds in S1 lignite ashes that react at an early stage period, while for less reactive S2 bituminous ashes those structure-forming reactions are shifted to later stages of curing. This can also be observed in SEM images Figure 7 and Figure 9 and will be partly discussed in further chapter.\u003c/p\u003e\n\u003cp\u003eWhile the coarser particles (C fraction) understandably had lower overall reactivity, especially at early stages, the strong initial strain development at 0-14 days can be observed for both S1.C and S2.C ashes. This can be related to the interlocking effect, where the angular shape of the Coarse grains contributes to mechanical interlocking between particles which manifested as reasonably high early strain test results [17,58,59]\u003c/p\u003e\n\u003cp\u003eThe medium fractions for both ash types S1.M and S2.M showed the overall lowest strength values, possibly because these particles were not large enough for a significant interlocking effect for the early-stage compressive strain gain, nor fine enough to contain sufficient reactive potential as in F and UF fractions. In addition, for the S2 ashes, the interlocking effect influence on structure-forming processes is lower compared to S1, due to the nature of grains shape which is predominantly spherical and smooth for S2 bituminous ashes. Bituminous coal combustion processes take place at higher temperatures which results in an increase in the amount of melted particles and a higher average smoothness and sphericity of grains [24,25].\u003c/p\u003e\n\u003cp\u003eIncreasing the amount of ash additives beyond a certain limit may negatively impact the final strain results. This negative effect may appear due to the absorption of free water essential for the hydration microstructure formation processes, however, curing in underwater conditions might eliminate this factor. Furthermore, increased ash content can result in a loss of workability, as was confirmed by rheological tests, leading to an insufficient settling of fresh mortars and incomplete structural continuity promoting the formation of cracks, pores, and internal stresses. Additionally, excessive ash content in the matrix can result in increasing non-reactive ash-to-ash interconnection clusters which impede strain development (Fig.6), particularly in the early stages when coarse particles are involved [60,61]. This effect can be observed in S2.C samples, where 40% ash addition results in a decrease of final strain compared to S2.C 30% resulting at 2.85 MPa and 1.71 MPa resp.\u003c/p\u003e\n\u003cp\u003eFor individual fly ash types and fractions, it is important to adjust the quantities and composition of additives to achieve the desired outcomes, as they may exhibit varying behaviors, leading to different results.\u003c/p\u003e\n\u003cp\u003e\u003cem\u003eFly Ash granulometry influence\u003c/em\u003e\u003c/p\u003e\n\u003cp\u003eThe microstructural studies sustain the compressive strain results, and there was a strong correlation observed between the obtained strain and microstructural results.\u003c/p\u003e\n\u003cp\u003eComparative analysis of the microscopic morphology (Fig.7, Fig.9, Fig.10) demonstrates that in the early period of 14 days, the spherical fly ash particles were still smooth, which indicates their relatively longer time reactivity, compared to high Ca-content grains and cement particles. The fly ash particles began to hydrate from the surface at later stages, so at 28 and 90 days the pits in the inert surface can be observed. Worth noticing is the lower particle dissolution level of S2 ashes compared to S1. This can be related to the higher Si content of S2 ashes, so those particles have longer activation and dissolution time. Figure 9 presents the reactivity rate of ashes at 90 days of curing depending on the EDS chemical content composition of the individual grain. The reactivity and solubility level increase with increasing structure modifiers content in particles, so the high silicious S2 ashes contribute lower reactivity compared to calcaneus S1 ashes. Also, for this reason, the S1 sample structure is denser, and more hydration products can be observed. [15,46,57,62]\u003c/p\u003e\n\u003cp\u003eIt was also observed a difference in microscale structure formation for S1 and S2 ashes, whereas, for the S1 sample, highly dense needle crystals are abundant. Those needle crystals are an Al-Ca-S-hydrated needle-shaped ettringite mineral crystals, formed in the presence of high concentrations of SO\u003csub\u003e4\u003c/sub\u003e\u003csup\u003e-2\u003c/sup\u003e and the presence of elevated CaO content (as in the case of S1 ashes) [63,64]. The formation of ettringite is enhanced by the high containment of Al oxides, available from mineral decompositions and amorphous phase. This contributes to the crystalline phase formation which affects the structure, as pores and free spaces become filled with needles. The ettringite formation can be responsible for the degradation of cementitious materials, through the swelling of the material followed by crack diffusion in the structure[63,65,66]. Gesoğlu et all. [67] show that for porous materials, such as fly ash clay-cement suspensions discussed in this study, ettringite crystal growth does not pose a risk of expansion cracking, because those crystals grow in pores and empty spaces in structure, causing an increase in final strain, structure tightness, and potentially causing an increase in permeability properties [68\u0026ndash;70]. So the highly reactive S1 particles start to dissolve and intersect with the surroundings, in a result filling the pores and creating a more dense structure compared to S2. For the S2 samples, mostly cement hydration phases are observed while ash particles remain unreacted.\u003c/p\u003e\n\u003cp\u003eWorth noticing is the influence of agglomerates and \u0026ldquo;pocket-enclosed\u0026rdquo; grains in S1.O and S2.O ashes (Fig. 10). These agglomerates cause formations of regions in the structure, where clusters of unreacted ashes are present, providing anisotropy to the structure. The pocket-enclosed grains result in the immobilization of some potentially reactive grains. Those effects cause the final strain to decrease for S1.O and S2.O ash suspensions. For other fractions, those effects have less impact because performed aerodynamic separation processes cause a disintegration effect, where low-durable grains and agglomerates undergo breakdown and ashes obtain a higher level of dispersion [39,40]. As a result, a higher amount of individual particles can be released and participate in structure formation. Fractionation has a significant impact on structure formation intensity , hydration processes and grain reactivity.\u003c/p\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eThe separation of fly ash into different size fractions results in fractions with varying chemical, mineralogical, and physical characteristics. Finer fractions contain increased levels of reactive aluminum, calcium, and sulphur compounds compared to coarser with more silica-rich content.\u003c/p\u003e\n\u003cp\u003eFiner ash fractions possess higher reactivity, evidenced by rapid viscosity increases upon water mixing as well as enhanced early strength development. The ultrafine fraction induced flash setting within a few minutes after mixing minutes. In contrast, coarse fractions showed more gradual reactivity behavior over longer timescales.\u003c/p\u003e\n\u003cp\u003eInteractions between the ashes and clay suspensions led to complex rheological impacts dependent on particle fineness, shape, and mineralogy. High calcium S1 ashes resulted in more intense early hydration reactions compared to siliceous S2 ashes.\u003c/p\u003e\n\u003cp\u003eMicrostructural analysis correlated the improved compressive strength of clay-cement mortars to the ability of fine ash fractions to accelerate the formation of denser, more uniform structures. The results of this work demonstrate the differences between individual fly ash fractions and their potential to engineer properties of suspension-based construction materials and systems.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAuthor Contributions:\u003c/strong\u003e JD contributed to conceptualization, methodology, validation, formal analysis, investigation, data curation, writing\u0026mdash;original draft, and visualization. PI and ŁW, contributed to methodology, validation, formal analysis, investigation, data curation, resources, writing\u0026mdash;review and editing, and supervision, AS \u0026ndash; writing, editing and supervision, MJ \u0026ndash; formal analysis\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding:\u003c/strong\u003e This research received no external funding.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eInstitutional Review Board Statement:\u0026nbsp;\u003c/strong\u003eNot applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eInformed Consent Statement:\u0026nbsp;\u003c/strong\u003eNot applicable.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflicts of Interest:\u003c/strong\u003e The authors declare no conflicts of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData Availability Statement:\u0026nbsp;\u003c/strong\u003eThe datasets used and/or analyzed during the current study available from the corresponding author on reasonable request\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eAlterary, S.S.; Marei, N.H. 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Relating Ettringite Formation and Rheological Changes during the Initial Cement Hydration: A Comparative Study Applying XRD Analysis, Rheological Measurements and Modeling. \u003cem\u003eMaterials\u003c/em\u003e \u003cstrong\u003e2019\u003c/strong\u003e, \u003cem\u003e12\u003c/em\u003e, 2957, doi:10.3390/ma12182957.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"
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