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Article Old Dumped as a Replacement in Composites

Jolanta Harasymiuk * and Andrzej Rudzi ´nski

Institute of Building , Faculty of Geodesy, Geospatial and Civil Engineering, University of Warmia and Mazury in Olsztyn, Heweliusza 4, 10-724 Olsztyn, Poland; [email protected] * Correspondence: [email protected]; Tel.: +48-89-523-4586

 Received: 30 December 2019; Accepted: 2 March 2020; Published: 31 March 2020 

Abstract: The use of industrial residues to replace natural resources for the production of building materials is economically and ecologically justified. Fly ash (FA) taken directly from electro-filters is commonly used as a cement replacement material. This is not the case, however, for old dumped fly ash (ODFA) that has been accumulating in on-site waste dumps for decades and currently has no practical use. It causes environmental degradation, which is not fully controlled by the governments of developed countries. The aim of the study was to assess the possibility of using ODFA as a partial replacement for sand in cement composites. ODFA replaced part of the sand mass (20% and 30%) in composites with a limited amount of cement (a cement-saving measure) and sand (saving non-renewable raw material resources). ODFA was activated by the addition of different proportions of hydrated , the purposes of which was to trigger a pozzolanic reaction in ODFA. The quantitative composition of the samples was chosen in such a way as to ensure the maximum durability and longevity of composites with a limited amount of cement. The 28-day samples were exposed to seawater attack for 120 days. After this period, the compressive strength of each sample series was determined. The results suggest the possibility of using ODFA with hydrated lime to lay town district road foundations and bike paths of 3.5 to 5 MPA compressive strength. What is more, these composites can be used in very aggressive environments.

Keywords: old dumped fly ash (ODFA); sand replacement; lime; durability of cement composites with ODFA

1. Introduction The 21st century is characterized by the desire to, potentially, fully implement sustainable growth in all areas of social and economic life. This trend also concerns the construction sector. Globally, in Europe and particularly in Poland, construction projects for enterprises that potentially significantly affect the environment always require an environmental impact assessment [1]. Moreover, a habitat assessment may precede the implementation of every construction project with a significant impact on the area or the areas incorporated in the ecological network Natura 2000 [2]. Both analyses of construction and material solutions for building structures, as well as environmental assessments of commercial buildings are common and are carried out in order to reduce their environmental impact [3–5]. However, in recent years, attitudes towards the design of building structures have changed. Presently, the should consider the effectiveness of solutions for the whole life spans of buildings [6,7]. Thus, the continuous search for new material solutions using industrial waste is necessary [8,9]. One example of this type of industrial waste is fly ash (FA), which is a dust collected in electro-filters after the combustion of hard or brown in the different combustion chambers of energy plants (e.g., power stations, heat and power plants). The overwhelming majority of FA is regained directly from production (FA from electro-filters). It is a valuable component of and

Buildings 2020, 10, 67; doi:10.3390/buildings10040067 www.mdpi.com/journal/buildings Buildings 2020, 10, x FOR PEER REVIEW 2 of 18 Buildings 2020, 10, 67 2 of 18 valuable component of cements and cement composites (mortars and ). However, a troublesome waste that spoils the natural environment is the FA that has for decades accumulated in on-sitecement waste composites dumps, (mortars often close and concretes).to urban area However,s. The widespread a troublesome phenomenon waste that of spoils depositing the natural by- productsenvironment of coal is the combustion FA that has at forfactory decades dumps accumulated is associated in on-sitewith the waste dominant dumps, mode often of close conventional to urban energyareas. The production. widespread The phenomenon main source of depositingelectricity and by-products heat in the of world coal combustion is still the combustion at factory dumps of hard is coalassociated and . with the Figure dominant 1 shows mode that of the conventional amount of energy FA produced production. in 2010–2017 The main sourcein Poland of electricity slightly decreased,and heat in whereas the world the is amount still the combustionof FA landfilled of hard cons coaliderably and lignite. increased Figure in 1the shows same that period the amount of time [10–17].of FA produced in 2010–2017 in Poland slightly decreased, whereas the amount of FA landfilled considerably increased in the same period of time [10–17].

Figure 1. Graph of quantitiesquantities of of fly fly ash ash (FA) (FA) produced produced and and deposited deposited on landfillson in Poland in Poland in 2010–2017. in 2010– 2017. This problem does not only apply to Poland [18,19]. As reported in [20], only a quarter of the total production of this waste is utilized. According to the Environmental Protection Agency (EPA), This problem does not only apply to Poland [18,19]. As reported in [20], only a quarter of the in the year 2008 FA was disposed of in over 310 active on-site landfills and 735 active on-site surface total production of this waste is utilized. According to the Environmental Protection Agency (EPA), impoundments. Landfills averaged over 120 acres in size and 40 feet in depth, while impoundment in the year 2008 FA was disposed of in over 310 active on-site landfills and 735 active on-site surface areas averaged over 50 acres in size and 20 feet in depth. With the dominance of the current mode impoundments. Landfills averaged over 120 acres in size and 40 feet in depth, while impoundment of conventional energy production and the poor tendency to utilize freshly produced FA, it can be areas averaged over 50 acres in size and 20 feet in depth. With the dominance of the current mode of assumed that the problem will not be reduced in the near future. Thus, new applications for ODFA, conventional energy production and the poor tendency to utilize freshly produced FA, it can be should be sought, which makes studies on this category of waste indispensable. assumed that the problem will not be reduced in the near future. Thus, new applications for ODFA, Scientific publications devoted to the use of ODFA in pastes, mortars or concretes are limited. should be sought, which makes studies on this category of waste indispensable. Up until now, there have been many publications concerning the usage of FA taken directly from Scientific publications devoted to the use of ODFA in pastes, mortars or concretes are limited. electro-filters. Such FA has been used mainly as a cement replacement. Only in recent years has the Up until now, there have been many publications concerning the usage of FA taken directly from potential for the partial replacement of cement by FA from electro-filters in concretes (up to 50% of electro-filters. Such FA has been used mainly as a cement replacement. Only in recent years has the cement mass) been discussed [21–23]. According to the PN-EN 206+A1:2016 standard [24], the share of potential for the partial replacement of cement by FA from electro-filters in concretes (up to 50% of FA in mortars and concretes may amount to up to 30% of the cement mass, meaning that the use of this cement mass) been discussed [21–23]. According to the PN-EN 206+A1:2016 standard [24], the share waste is in the range of 100–120 kg/m3. Our study develops the use of ODFA as a partial replacement of FA in mortars and concretes may amount to up to 30% of the cement mass, meaning that the use for sand (20% and 30% of sand mass) in cement composites. It involves the use of this waste in the of this waste is in the range of 100–120 kg/m3. Our study develops the use of ODFA as a partial range of 300–400 kg m3. replacement for sand/ (20% and 30% of sand mass) in cement composites. It involves the use of this Due to its lack of binding capacity, FA requires the use of certain additives to serve as binding waste in the range of 300–400 kg/m3. activators.Due to In its [ 25lack], sodium of binding sulphate capacity, was FA used requires as a binding the use activator, of certain whereas additives in [ 26to], serve a paste as binding with FA activators.was activated In [25], with sodium sodium sulphate hydroxide. was used In [27 as], calciuma binding hydroxide activator, madewhereas up in 9.4% [26], of a the paste paste with mass FA wasas an activated activator with for asodium paste with hydroxide. FA. The In amount [27], calc ofium hydroxide used inmade our up study 9.4% ranged of the frompaste0.31% mass as to an0.92% activator and from for 0.46%a paste to with 1.31% FA. of theThe composites’ amount of mass,calcium respectively used in our (the study remaining ranged part, from made 0.31% up to of 0.92%lime, came and from the0.46% hydration to 1.31% of of the and composites’ in cement). mass, respectively These amounts (the dependedremaining onpart, the made assumed up ofcontent lime, ofcame ODFA from in the composites.hydration of Our alite previous and belite study in cement). (unpublished) These showedamounts that depended this amount on the of assumedcalcium is content optimal of when ODFA considering in the composites. the compressive Our previous strength study of the (unpublished) standard sample showed (28 days) that andthis the prolonged sample (148 days). Buildings 2020, 10, 67 3 of 18

The use of any kind of FA to produce cement composites is reasonable only in the case of obtaining the assumed technological properties of such materials, and first of all, durability. The problem of durability of cement composites was the subject of numerous publications [28–31]. The reason for that is the high pollution level of the atmosphere and , which increases the aggressiveness of the environment and the speed of corrosion. In the publications referred to, however, mainly the durability of was dealt with. In our research, we dealt with the durability of composites with a considerable addition of ODFA (240% and 360% of cement mass). The most frequent aggressions are chlorides (the sources of chloride salts are defrosting agents and sea water) and . The influence of chloride salt activity on building mortars with FA corresponding to the PN-EN 450:2012 standard [32] was examined in [33,34]. Permeation of chloride to concrete was examined in [35]. The impact of ion activity on concretes was examined in [36–40]. Seawater is a more complex corrosive agent than the above-mentioned agents. It contains a series of salts (mainly chlorides and sulphates) that work simultaneously. In [41] the influence of various aggressive solutions, namely HCl, Na2SO4 and seawater, on cement pastes and mortars was monitored. The activity of seawater on cement pastes without addition of FA was examined in [42]. However, the concentration of the aggressive media in these publications was low. In our research, we dealt with the effect of seawater on technological properties of cement composites with a large amount of ODFA. Seawater had a salinity of 4.3%. According to [29], such salinity is high, more than two times higher in comparison to other studies [43]. The assumed concentration of seawater solution led to an intensified process of aggression. Summing up, there are no publications devoted to the usage of ODFA as an ingredient of cement composites. There is also a lack of publications pertaining to the durability of such composites in very aggressive environments. The aim of this study was to evaluate the possibility of using the highest amount of useless energy-producing waste material (ODFA) as a partial replacement of sand in cement composites. Using ODFA reduces degradation of the natural environment caused by storage of FA and can solve the problem that the governments of developed countries fail to manage. The composites under study contained a small amount of cement (25% of the standard mass) and a large proportion of ODFA (240% and 360% of the mass of the used cement). A partial replacement of sand with ODFA in cement composites would decrease the demand of the road building materials market for this non-renewable raw material. A reduction of cement content in composites is connected to a decrease in emissions of the CO2 related to its production.

2. Materials and Methods

2.1. Materials In this study, locally available building materials were used. Table1 shows the quantitative and qualitative characteristics of these materials. From the examined ODFA, natural sand of the grain size of 0–2 mm, and , a series of sand–ash–cement composites were made, the qualitative and quantitative composition of which are shown in Table2. Buildings 2020, 10, 67 4 of 18

Table 1. Characteristics of the materials used in the research.

Materials Quantitative and Qualitative Characteristics The petrographic composition of sand was classified according to the Natural sand with grain size of 0–2 PN-EN 932-3:1999 standard [44]. The sand contained 80.9% of , mm obtained from Eco-Ter in chalcedony and opal, 12.5% of magma and metamorphic rocks and Kronowo (Poland) pit 6.6% of sedimentary rocks. The alkaline reactivity was 0. The loss of ignition of ca. 15% classified according to the PN-EN ODFA obtained from Michelin S.A. 196-2:2013-11 standard [45], granulation containing ca. 20% of the up Company (Poland) to 0.045 mm fraction, yet not containing unbound calcium. CEM I-32, 5R Portland cement The Portland cement was classified according to the PN-EN 197-1:2012 obtained from the O˙zarów cement standard [46]. plant (Poland) The lime was classified according to the PN-EN 459-1:2015-06 Hydrated lime obtained from Natura standard [47]. Its content was CaO + MgO 95.2%, MgO 0.7%, CO production facility (Poland) 2 1.8%, Ca(OH)2 91.4%, SO3 0.1%, H2O 0.8%. Composition of seawater solution consisted of (in 1 dm3) 30.1 g NaCl, Seawater solution 6.0 g MgCl2, 5.0 g MgSO4, 1.5 g CaSO4, 0.2 g KHCO3 (p.a.), according to [29]. Distilled water -

Table 2. The qualitative and quantitative composition of the composites.

3 3 3 3 3 Series Cement (kg/m ) Sand (kg/m ) ODFA (kg/m ) Water (kg/m ) Ca(OH)2 (kg/m ) 0 * 136.3 1639.0 - 267.1 -

2H0 132.9 1288.4 319.1 307.3 -

2H2 130.2 1250.2 312.5 306.8 6.3

2H4 124.7 1196.9 299.2 299.2 12.0

2H6 120.3 1155.6 288.9 294.3 17.3

3H0 132.3 1111.8 476.4 329.4 -

3H2 129.0 1083.9 464.5 326.9 9.3

3H4 127.1 1067.9 457.7 327.7 18.3

3H6 123.0 1065.7 442.7 322.4 26.6 * Control sample.

As the “0” series, the qualitative composition close to the standard mortar was assumed (used to determine cement classes), but the standard sand was replaced with natural sand and the mass of cement was decreased by 75% (from 450 g according to PN-EN 196-1:2006 [48] to 112.5 g). In the composites, 20% and 30% of the mass of sand was replaced by ODFA. The composites were activated by the addition of hydrolyzed lime in the amount of 0%, 2%, 4% and 6% of the mass of the added ODFA (series “2H0”, “2H2”, “2H4”, “2H6”, “3H0”, “3H2”, “3H4”, “3H6”) (Activation of FA can be carried out with two methods, mechanical and chemical. The mechanical method consists in the fragmentation of FA [49] and is expensive. Chemical activation is achieved by the addition of activators to the composite, e.g. calcium hydroxide [50], sodium sulphate [25] and [26]. Chemical activation using calcium hydroxide was applied in the work.) This was done because ODFA is a that has no binding properties but rather reacts with Ca (OH)2 formed during the hydration of alite and belite from cement. With a limited amount of cement in 3 composites (from 124.7 to 132.9 kg/m ), an insufficient amount of Ca (OH)2 is formed (assuming that the cement contained about 55% alite and about 12% belite). The insufficient amount of Ca(OH)2 in the composites had to be replenished. Buildings 2020, 10, 67 5 of 18

2.2. Sample Preparation The samples of ODFA were taken from the heap located nearby the Michelin-Polska factory in Olsztyn (Poland), from a depth of ca. 1 m. The ingredients of fresh mixtures were blended in a laboratory concrete-mixer (according to the PN-EN 196-1:2006 standard [48]). The volume of water in individual series of these mixtures was determined experimentally to obtain a dense– consistency. The consistency of fresh mixtures was examined on a flow table according to the PN-EN 1015-3:2000/A1:2005 standard [51]. The consistency was determined at a flow of 12 0.5 cm. ± Then, cylindrical specimens were made with dimensions of 80 mm in diameter and 80 mm in height. All specimens were compacted in a Proctor device. After demolding, all specimens were transferred to the moisture chamber and kept at a relative of 97% 3% and a temperature of 20 2 C, ± ± ◦ until their testing age (28 days). After this time, part of each specimen was left in the moisture chamber for 120 days. A second part was submerged in distilled water, and a third part was submerged in the seawater solution for 120 days.

2.3. Testing Methods The assumed scope of the research consisted of both ODFA and hardened composites tests. To determine the usefulness of ODFA as a partial sand replacement, conventional (grain size analysis, loss on ignition (LOI) determination) and modern research techniques (thermal analysis, scanning microscopy, electronic spectroscopy) were applied. LOI determination was conducted according to the PN-EN 196-2:2013-11 standard [45]. Dried at 105 ◦C, the specimens were calcined at 950 ◦C. The percentage of organic matter (unburned ) was determined from the weight loss (the average value is presented in this work). The test using the TGA–DTA thermal analysis of chemical processes in ODFA was made on a simultaneous TGA–DTA type SDT 2960 thermoanalyzer (TA Instruments). The thermogram was registered in atmospheric air with the speed of warming of 10 ◦C/min to 1000 ◦C. This test was made in the Chemical Analysis Laboratory of the Nicolaus Copernicus University in Toru´n(Poland). The test of ODFA structure was conducted with the help of scanning electronic microscopy (SEM). The observation was done with a JSM-5310LV scanning . The EDS analyses of ODFA were made with the aid of an SA Ranger spectrometer with a XFLASH detector. The above-mentioned tests enabled physico-chemical characterization of ODFA. Tests of hardened composites included density, weight water absorption and standard and long-term compressive strength. Tests for density and water absorption were done for all the 28-day sample series. The compressive strength of the composites with ODFA was determined after 28 days of setting and hardening, according to the PN-EN 14227-3:2004 standard [52]. To determine the durability of the composites, the 28-day samples were subjected to a very aggressive environment. They were submerged in a seawater solution for 120 days. For comparison, the successive sample series were submerged in distilled water and in a moisture chamber for 120 days. The results of the activity of the seawater solution and the distilled water on the composites were determined on the basis of a measurement of compressive strength according to the PN-EN 14227-3:2004 standard [52]. The structure of the samples after seawater attack was examined with the aid of a JSM-5310LV scanning microscope.

3. Results

3.1. Old Dumped Fly Ash Tests The results of ODFA tests are shown in Figure2, Figure3, Figures4 and5a–c and Table3. Buildings 2020, 10, 67 6 of 18

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FigureFigure 2. 2. Curve Curve of of ODFA ODFA grain grain size. size. Figure 2. Curve of ODFA grain size. Figure 2. Curve of ODFA grain size.

FigureFigure 3. ThermalThermal 3. Thermal analysis—TG analysis—TG analysis—TG and and and DTA DTADTA curves curvescurves of of OD OD ODFA;FA;FA; thethe the greengreen green curve curve (TG)(TG) (TG) representsrepresents represents the the the Figurechangechangechange 3. in massThermal in mass of of the the ofanalysis—TG samplethe sample sample in in temperature in temperature andtemperature DTA functicurves function; function; on;of the the OD blue blue blueFA; curve curvethe curve green (TGA)(TGA) (TGA) curverepresents represents (TG) the the represents change the change change of of the of changetemperaturetemperaturetemperature in mass of the of of the sample samplethe sample sample in in regard regardin regardtemperature to to theto the the reference reference reference functi on;sample. sample.sample. the blue curve (TGA) represents the change of temperature of the sample in regard to the reference sample.

FigureFigure 4. SEM 4. SEM image image of of ODFA; ODFA; points points 1–41–4 representrepresent selected selected points points for for EDS EDS analysis. analysis. Figure 4. SEM image of ODFA; points 1–4 represent selected points for EDS analysis. Figure 4. SEM image of ODFA; points 1–4 represent selected points for EDS analysis. Buildings 2020, 10, 67 7 of 18 Buildings 2020, 10, x FOR PEER REVIEW 7 of 18

(a)

(b)

(c)

FigureFigure 5. 5.( a(a)) EDS EDS analysis analysis of of ODFA ODFA in in the the point point 1 1 in in Figure Figure4;( 4;b ()b EDS) EDS analysis analysis of of ODFA ODFA in in the the point point 2 in2 Figurein Figure4;( 4;c) ( EDSc) EDS analysis analysis of ODFAof ODFA in thein the point point 2 in 2 Figurein Figure4. 4.

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Table 3. The oxide composition of ODFA.

Oxide Content (%)

SiO2 40.46

Al2O3 25.00

Fe2O3 10.21 CaO 9.81 MgO 2.44

SO3 0.25

K2O 0.26

Na2O 0.49

P2O5 0.21

TiO2 1.21 MnO 0.15 SrO 0.04

The fineness of FA had a considerable influence on its [53]. The fractions below 45 µm were characterized by strong Pozzolanic activity. Figure2 shows that the fractions up to 45 µm made up less than 20% in the examined ODFA. Hence, because of fineness, ODFA was not in accordance with the PN-EN 450-1:2012 standard [32]. A property of FA that is important from the practical point of view is LOI. The result of a high LOI is an enhanced water demand of FA (compared to FA of low losses) [53]. According to the PN-EN 450-1:2012 standard [32], it should be 5%, while in our research it was 15%. A supplement to the above-mentioned test was a more detailed TGA–DTA analysis (Figure3). As seen in Figure3, ODFA contained 3.025% of H 2O and 12.76% of organic matter, mainly of coal. Both mentioned tests showed that the content of unburnt coal in ODFA significantly surpassed the amount accepted in concretes. The results of the morphological observation of ODFA are presented in Figure4. A microscopic observation was made at a magnification of 200x. The SEM image showed that examined ODFA was fine-grained. The majority of the grains were spherical, with a smooth surface and a diameter up to 45 µm. The EDS analyses of ODFA showed the presence of a number of elements in marked points (Figure5a–c). The maximum values were recorded for Si and Al. This corresponds to the content of their oxides (SiO2 and Al2O3) given in Table3. A spectrographic analysis showed the qualitative and quantitative composition of ODFA. The presented results were average values from three tests. Based on the content of the three basic oxides (SiO2, Fe2O3, Al2O3), it was determined that the ODFA examined was a siliceous FA (Table3). ODFA used in the research did not meet the requirements of the PN-EN 450-1:2012 standard [32] because of its losses on ignition and its fineness. However, there have been contradictory research results concerning the influence of high ignition losses on compressive strength of composites with FA [22].

3.2. Cement Composite Tests

3.2.1. Compressive Strength before and after Seawater Attack All the specimens were examined for compressive strength after 28 and 148 days of setting and hardening. Table4 presents the results of this test. Buildings 2020, 10, 67 9 of 18

Table 4. Results of the compressive strength of the 28-day and 148-day samples as well as the 28-day samplesBuildings 2020 after, 10 120, x FOR days PEER of submersionREVIEW in distilled water and seawater. 9 of 18

Table 4. Results of the compressive strengthCompressive of the 28-day Strength and 148-day (MPa) samples as well as the 28-day samples after 120 days of submersion in distilled water and seawater. 28 Days 28 + 120 Days 28 + 120 Days 28 + 120 Days Series in a Moisture Chamber inCompressive a Moisture Chamber Strength in(MPa) Distilled Water in Seawater 028 1.85Days 28 + 1.95120 Days 28 + 2.02 120 Days 28 + 120 1.68 Days Series 2H0 in a Moisture1.90 Chamber in a Moisture 2.20 Chamber in Distilled 2.20 Water in Seawater 2.05 0 1.85 1.95 2.02 1.68 2H2 3.62 4.90 3.50 3.07 2H0 1.90 2.20 2.20 2.05 2H4 4.21 5.40 3.65 3.12 2H2 3.62 4.90 3.50 3.07 2H6 4.34 5.25 3.44 3.85 2H4 4.21 5.40 3.65 3.12 3H2H06 4.342.00 2.20 5.25 2.25 3.44 2.20 3.85

3H20 2.003.90 5.722.20 3.062.25 3.502.20

3H42 3.905.00 6.20 5.72 3.56 3.06 3.72 3.50 3H4 5.00 6.20 3.56 3.72 3H6 5.07 5.90 3.78 3.63 3H6 5.07 5.90 3.78 3.63

FigureFigure6a,b 6a,b show show an erroran error bar bar depicting depicting the the standardstandard (28-day) and and the the long-term long-term (148-day) (148-day) compressivecompressive strength strength of theof the series series of of composites composites keptkept in a moisture moisture chamber. chamber.

(a)

(b)

Figure 6. Cont. Buildings 2020, 10, x FOR PEER REVIEW 10 of 18

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(c(c) ) Figure 6. (a) Compressive strength data of the 28-day series of composites kept in a moisture chamber; FigureFigure 6. (a) 6. Compressive (a) Compressive strength strength data data of of the the 28-day 28-day seriesseries of of composites composites kept kept in ina moisture a moisture chamber; chamber; (b) Compressive(b) Compressive strength strength data data of of thethe 148-day148-day seriesseries of of composites composites kept kept in a in moisture a moisture chamber; chamber; (c) (c) (b) Compressive strength data of the 148-day series of composites kept in a moisture chamber; CompressiveCompressive strength strength data data of of the the 148-day 148-day seriesries of of composites composites kept kept in seawater.in seawater. (c) Compressive strength data of the 148-day series of composites kept in seawater. Figure 6c shows an error bar depicting the long-term (148-day) compressive strength of the series FigureFigure6c 6c shows shows an an error error bar bar depicting depicting the the long-term long-term (148-day) (148-day) compressive compressive strength strength of of the the series series of compositesof composites kept kept in inseawater seawater solution. solution. Each boxbox in in Figure Figure 6a–c 6a–c represents represents the compressivethe compressive strength strength of compositesof 6 separate kept specimens. in seawater The solution. dots correspond Each box to the in Figuremean value;6a–c representsthe lines show the standard compressive deviation. strength of 6 separate specimens. The dots correspond to the mean value; the lines show standard deviation. of 6 separateFigure specimens. 7 shows that The all dots the correspondseries of samples to the with mean ODFA value; and the lime lines gained show a higher standard compressive deviation. FigurestrengthFigure7 shows 7after shows 28 that days that all in all thecomparison the series series of to of samples the samples control with with sample. ODFA ODFA and and lime lime gained gained a highera higher compressive compressive strengthstrength after after 28 28 days days in in comparison comparison to to the the control control sample. sample.

Figure 7. The changes in the compressive strength of the 28-day samples in comparison to the compressive strength of the control sample (the samples kept in a moisture chamber).

Figure 7. The changes in the compressive strength of the 28-day samples in comparison to the The maximum increase of compressive strength was observed in the “3H4” and “3H6” series of compressiveFigure 7. The strength changes of the in control the compressive sample (the strength samples of kept the in 28-day a moisture samples chamber). in comparison to the samples,compressive which strength amounted of the to control270.2% sampleand 274.1%, (the samples respectively. kept in a moisture chamber). The maximumThe results increase of 120-day of compressiveinfluence of the strength seawater was solution observed on composites in the “3H4” with and ODFA “3H6” and serieslime of are shown in Figure 8. samples,The which maximum amounted increase to 270.2% of compressive and 274.1%, strength respectively. was observed in the “3H4” and “3H6” series of samples,The results which of amounted 120-day influence to 270.2% of and the seawater274.1%, respectively. solution on composites with ODFA and lime are shownThe in Figure results8. of 120-day influence of the seawater solution on composites with ODFA and lime are shown in Figure 8. Buildings 2020, 10, x FOR PEER REVIEW 11 of 18 Buildings 2020, 10, 67 11 of 18 Buildings 2020, 10, x FOR PEER REVIEW 11 of 18

Figure 8. The changes of the compressive strength of the composite samples with ODFA and lime in Figure 8. The changes of the compressive strength of the composite samples with ODFA and lime in Figurecomparison 8. The to changes the samples of the without compressive lime subjected strength ofto ththee compositeinfluence of samples seawater with solution ODFA for and 120 lime days. in comparison to the samples without lime subjected to the influence of seawater solution for 120 days. comparison to the samples without lime subjected to the influence of seawater solution for 120 days. TheseThese results results were were determined determined on on the the basis basis of of the the compressive compressive strength strength measurement measurement and and were were comparedcomparedThese with withresults the the compressivewere compressive determined strength strength on the of of samplesbasis sample of the withs with compressive the the same same composition strengthcomposition measurement but but not not subjected subjected and were to to seawatercomparedseawater aggression. aggression. with the compressive “2H0” “2H0” and and “3H0”series strength“3H0”series of containingsample containings with ODFA ODFA the same (but (but without composition without lime) lime) but practically practically not subjected did did not not to changeseawaterchange their their aggression. compressive compressive “2H0” strength. strength. and “3H0”series However, However, this containing strengththis strength wasODFAvery was (but lowvery without and low amounted andlime) amounted practically to about to did 2MPa about not (2.05change2MPa and (2.05 their 2.20 MPa).andcompressive 2.20 The MPa). strength strength. The of strength the However, “0” sampleof the this “0” decreased strength sample bywas decreased 13.8%. very Thelow by compressive and13.8%. amounted The strengthcompressive to about of the2MPastrength “3H0” (2.05 seriesof theand did“3H0” 2.20 not MPa). series change, Thedid and notstrength “2H0”change, of decreased andthe “0”“2H0” sample by decreased 6.8%. decreased Series by “2H2”6.8%. by 13.8%.Series and “2H4” “2H2”The compressive and and “3H2” “2H4” andstrengthand “3H4” “3H2” of obtained theand “3H0” “3H4” similar series obtained values did notsimilar (from change, 3.07values and to 3.72(from “2H0” MPa). 3.07 decreased Theirto 3.72 compressive MPa).by 6.8%. Their Series strength compressive “2H2” dropped and strength “2H4” by 57.8%anddropped “3H2” and 62.6%,by and 57.8% respectively.“3H4” and obtained 62.6%, Larger respectively. similar differences values Larger in(from decreases differences 3.07 to of 3.72 compressive in MPa).decreases Their strength of compressivecompressive were noted strengthstrength for thedroppedwere “2H6” noted andby for57.8% “3H6” the and“2H6” series, 62.6%, and amounting respectively.“3H6” series, to 61.5% Largeramounting and differences 73.3%, to 61.5% respectively. in anddecreases 73.3%, of respectively. compressive strength were noted for the “2H6” and “3H6” series, amounting to 61.5% and 73.3%, respectively. 3.2.2.3.2.2. Density Density 3.2.2. Density AA density density test test is ais basic a basic examination examination conducted conducted on all on building all building materials. materials. Figure Figure9 shows 9 anshows error an barerror depictingA bar density depicting the test density isthe a densitybasic of all theexamination of compositesall the composites conducted series afterseries on 28all after daysbuilding 28 of days binding materials. of binding and setting.Figure and setting.9 Each shows boxEach an representserrorbox represents bar thedepicting density the densitythe of density four of separate four of all separate the specimens. composites specimens. series after 28 days of binding and setting. Each box represents the density of four separate specimens.

FigureFigure 9. 9.Density Density data data of of the the 28-day 28-day series series of of composites. composites. Figure 9. Density data of the 28-day series of composites. Buildings 2020, 10, x FOR PEER REVIEW 12 of 18

Buildings 2020, 10, 67 12 of 18 BuildingsFigure 2020, 10, xshows FOR PEER the REVIEW changes of the density measurements of all the composite series after12 of 2818 days of binding and setting. FigureFigure 10 10 shows shows the the changes changes of theof the density density measurements measurements of all of the all composite the composite series series after 28 after days 28 ofdays binding of binding and setting. and setting.

Figure 10. Increase in density of the composite samples with ODFA and lime in comparison to the control sample. Figure 10. Increase in density of the composite samples with ODFA and lime in comparison to the Figure 10. Increase in density of the composite samples with ODFA and lime in comparison to the control sample. 3 controlThe density sample. of composites with ODFA ranged from 1628 to 1756 kg/m (samples “2H’’) and from 3 3 1647The to density1705 kg/m of composites (samples with“3H”). ODFA The ranged“0” sample from without 1628 to 1756 ODFA kg/ mhad3 (samples a density “2H”) of 1808 and kg/m from . 1647Generally, toThe 1705 density the kg /“3H”m of3 (samplescomposites samples “3H”).had with a slightly ODFA The “0” rangedlower sample density from without 1628 than to ODFAthe 1756 “2H” kg/m had samples.3 a (samples density “2H’’) of 1808 and kg /fromm3. Generally,1647 to 1705 the “3H”kg/m3 samples (samples had “3H”). a slightly The lower“0” sample density without than the ODFA “2H” samples.had a density of 1808 kg/m3. Generally,3.2.3. Water the Absorption “3H” samples had a slightly lower density than the “2H” samples. 3.2.3. WaterWeight Absorption of water absorption was determined by the ratio of the weight of absorbed water to the 3.2.3. Water Absorption weightWeight of the of specimen water absorption in the dry was state. determined Some stan bydards the ratio require of thethat weight the wate ofr absorbed absorption water of concrete to the weightbe limitedWeight of the up specimenof to water a certain absorption in the level dry (4%). state.was determinedThis Some is standards often by a thedifficult require ratio ofcondition that the the weight water to beof absorption obtainedabsorbed in ofwater industrial concrete to the beweightproduction, limited of upthe not tospecimen aonly certain for in concretes level the dry (4%). state. [54]. This Some is often standards a diffi requirecult condition that the to wate ber obtained absorption in industrialof concrete production,be limitedIt is known notup to only a that certain for concretesthe levelabsorption (4%). [54]. This of cementis often paa difficultste (assuming condition nonabsorbability to be obtained of in )industrial production,dependsIt is known on notthe that onlyamount the for absorption ofconcretes cement, of[54]. W/C cement ratio paste and (assuming degree of nonabsorbabilitycement hydration of (maturation aggregate) depends time and onconditions). theIt amount is known Figure of cement, that 11 theshows W /Cabsorption ratio an anderror degreeof barcement depict of cement paingste hydrationthe(assuming weight (maturation nonabsorbabilityof water timeabsorption and of conditions). aggregate)of all the Figuredependscomposite 11 shows on series the anamount after error 28 barof days cement, depicting of binding W/C the ratio weight and and setting of degree water. Each absorptionof boxcement represents hydratio of all the then composite (maturation density of series 4 time separate after and 28conditions).specimens. days of binding TheFigure results and 11 setting. ofshows determination Each an boxerror represents barof weight depict the ofing densitywater the weightabsorption of 4 separate of waterof specimens.the absorptionexamined The composites resultsof all ofthe determinationcompositeare presented series of in weight Figureafter 28 of12. days water of absorption binding and of thesetting examined. Each box composites represents are the presented density in of Figure 4 separate 12. specimens. The results of determination of weight of water absorption of the examined composites are presented in Figure 12.

FigureFigure 11. 11.Water Water absorption absorption data data of of the the 28-day 28-day series series of of composites. composites.

Figure 11. Water absorption data of the 28-day series of composites. Buildings 2020, 10, 67 13 of 18 Buildings 2020, 10, x FOR PEER REVIEW 13 of 18

FigureFigure 12. 12.Increase Increase in in water water absorption absorption of of the the 28-day 28-day series series of compositesof composites with with ODFA ODFA and and lime lime in comparisonin comparison to the to the control control sample. sample.

TheThe water water absorption absorption value value of of the the samples samples with with ODFA ODFA was was considerably considerably higher higher than than the the water water absorptionabsorption valuevalue ofof the the control control sample sample without without limelime andand ODFA.ODFA. For For the the “2H” “2H” samples samples the the increase increase waswas from from 44.1% 44.1% to to 63.8%. 63.8%. For For the the “3H” “3H” samples,samples, thethe increaseincrease waswas stillstill higherhigher andand rangedranged fromfrom 58.2%58.2% toto 74.5%.74.5%.

4.4. DiscussionsDiscussions TheThe ODFA ODFA used used in in the the research research did did not not meet meet the the requirements requirements of the of PN-ENthe PN-EN 450-1:2012 450-1:2012 standard standard [32] because[32] because of fineness of fineness and LOI.and LOI. Despite Despite this fact,this fact, theuse the ofuse it of in it composites in composites with with reduced reduced quantities quantities of cementof cement gave gave advantageous advantageous results. results. With aWith very a limited very limited quantity quantity of cement of incement the hydration in the hydration reaction, therereaction, was anthere insu wasfficient an insufficient amount of calciumamount hydroxideof calcium for hydroxide a Pozzolanic for a reaction Pozzolanic to occur. reaction The to applied occur. ODFAThe applied contained ODFA virtually contained no unbound virtually calcium no unbound oxide. Thecalcium ODFA oxide. content The in ODFA all the content examined in seriesall the ofexamined the samples series considerably of the samples exceeded considerably the cement exce content.eded the To cement make acontent. Pozzolanic To make reaction a Pozzolanic of ODFA possible,reaction theof ODFA additive possible, calcium the hydroxide additive incalcium the amount hydroxide of 0%, in 2%, the 4%, amount or 6% of of 0%, the 2%, mass 4%, of or ODFA 6% of was the suppliedmass of ODFA to each was of the supplied series ofto samples.each of the series of samples. ConsiderableConsiderable increasesincreases in the compressive compressive strength strength of of composites composites with with ODFA ODFA were were obtained obtained for forthe the 148-day 148-day samples samples as ascompared compared to the to the 28-day 28-day samples. samples. In the In thesamples samples with with ODFA ODFA and and lime, lime, the theincrease increase of compressive of compressive strength, strength, as compared as compared to the to strength the strength of the ofcontrol the control sample sample only with only ODFA, with ODFA,went up went from up 116.4% from 116.4% to 146.7%. to 146.7%. TheThe presence presence of of a a large large amount amount of of ODFA ODFA reduced reduced the the density density of of composites composites from from 6.7% 6.7% to to 12.8%. 12.8%. TheThe high high increase increase in in water water absorption absorption was was determined determined by the by presence the presence of a large of a amount large amount of ODFA of inODFA the composites in the composites [53]. ODFA [53]. bound ODFA water bound more water intensively more intensively than the than sand the it replaced. sand it replaced. TheThe seawater seawater solution solution applied applied in thein teststhe tests contains cont salts,ains whichsalts, mostwhich often most are often harmful are toharmful building to materials.building materials. The chloride The salts, chloride which salts, are awhich significant are a ingredient significant of ingredient seawater, canof seawater, act adversely can onact theadversely cement on matrix. the cement The deterioration matrix. The of deterioration technological of properties technological of cement-based properties compositesof cement-based and compositescomposites with and ODFAcomposites due to with aggressive ODFA activitydue to aggre of seawaterssive activity is connected of seawater with a transferis connected of reacting with a ionstransfer to the of place reacting of reaction, ions to i.e., the to place the interior of reaction, of a material. i.e., to the It caninterior occur of as a a material. result of twoIt can mechanisms: occur as a resultmigration of two mechanisms: and influx to the interior of a composite resulting from capillary pull [55], − − ionmigration diffusion and resulting influx to from the theinterior strength of a composite gradient in resulting its different from areas capillary [56]. pull [55], − − ion diffusion resulting from the strength gradient in its different areas [56]. The first mechanism gives a much higher speed of transport, which triggers a quick aggression process.The The first role mechanism of large capillary gives a much pores higher in the accelerationspeed of transport, of aggression which istriggers obvious. a quick The coeaggressionfficient ofprocess. diffusion The D role decreases, of large and capillary the solution pores strengthin the acce ofleration salts C increasesof aggression with is time, obvious. which The is causedcoefficient by theof diffusion progressive D decreases, hydration and of cementthe solution [57]. strength While assessing of salts C the increases process with of migration time, which in ais hardenedcaused by cementthe progressive paste, and hydration probably of also cement in an [57]. ash–cement While assessing paste, itthe should process be of borne migration in mind in thata hardened this is cement paste, and probably also in an ash–cement paste, it should be borne in mind that this is not pure diffusion. Diffusing ions react with the phases of the paste and are subject to absorption on the Buildings 2020, 10, x FOR PEER REVIEW 14 of 18 amorphous surface of the C–S–H phase. Chloride ions also react with hydrated calcium aluminate, giving Friedl’s salt C3ACaCl210H2O. This compound does not cause expansion, but on the contrary, it decreases the amount of expansive compounds created [28,42,56,58]. Chloride aggression to which Buildings 2020, 10, 67 14 of 18 composites with ODFA were exposed diminished their compressive strength. Simultaneous action Buildingson the mixtures 2020, 10, x ofFOR calcium PEER REVIEW and chloride salts, as well as magnesium sulphate, caused14 of the 18 notdecrease pure of di ffcompressiveusion. Diffusing strength ions in react all the with series the of phases the samples of the with paste ODFA and are and subject lime. toHowever, absorption the amorphous surface of the C–S–H phase. Chloride ions also react with hydrated calcium aluminate, onobtained the amorphous compressive surface strength of the of C–S–Hthe samples phase. with Chloride ODFA ions and also lime react after with seawater hydrated attack calcium was giving Friedl’s salt C3ACaCl210H2O. This compound does not cause expansion, but on the contrary, aluminate,definitely higher, giving Friedl’sby 49.8% salt to C87.8%,ACaCl than10H theO. compressive This compound strength does of not the cause “2H expansion,0” and“3H0 but” samples on the it decreases the amount of expansive3 compounds2 2 created [28,42,56,58]. Chloride aggression to which contrary,without lime. it decreases The composites the amount with of ODFA expansive and compoundslime, under createdthe influence [28,42, 56of, 58seawater]. Chloride attack, aggression created composites with ODFA were exposed diminished their compressive strength. Simultaneous action tomore which distinct composites and compact with ODFA crystals were (Figures exposed 13b, diminished 14b), than theirthe samples compressive with ODFA strength. but Simultaneous without lime on the mixtures of calcium and magnesium chloride salts, as well as magnesium sulphate, caused the action(Figures on 13a, the 14a). mixtures of calcium and magnesium chloride salts, as well as magnesium sulphate, decrease of compressive strength in all the series of the samples with ODFA and lime. However, the caused the decrease of compressive strength in all the series of the samples with ODFA and lime. obtained compressive strength of the samples with ODFA and lime after seawater attack was However, the obtained compressive strength of the samples with ODFA and lime after seawater definitely higher, by 49.8% to 87.8%, than the compressive strength of the “2H0” and“3H0” samples attack was definitely higher, by 49.8% to 87.8%, than the compressive strength of the “2H ” and“3H ” without lime. The composites with ODFA and lime, under the influence of seawater attack,0 created0 samples without lime. The composites with ODFA and lime, under the influence of seawater attack, more distinct and compact crystals (Figures 13b, 14b), than the samples with ODFA but without lime created more distinct and compact crystals (Figures 13b and 14b), than the samples with ODFA but (Figures 13a, 14a). without lime (Figures 13a and 14a).

(a) (b)

Figure 13. (a) SEM image of the 2H0 sample after seawater attack; (b) SEM image of the 2H6 sample after seawater attack.

These differences in the structure of the samples probably influenced the significant differences in these samples’ compressive strengths. In terms of the composition of the seawater solution, beside (a) (b) the principal salt, NaCl, it also contained MgCl2 and MgSO4 magnesium salts, which caused not only a sulphateFigure aggression, 13. (a) SEM image but also of the a magnesium 2H0 sample after one. seawater attack; ( b) SEM image of the 2H6 sample after seawater attack.

These differences in the structure of the samples probably influenced the significant differences in these samples’ compressive strengths. In terms of the composition of the seawater solution, beside the principal salt, NaCl, it also contained MgCl2 and MgSO4 magnesium salts, which caused not only a sulphate aggression, but also a magnesium one.

(a) (b)

Figure 14. (a) SEM image of the 3H0 sample after seawater attack; (b) SEM image of the 3H6 sample after seawater attack.

These differences in the structure of the samples probably influenced the significant differences in these samples’ compressive strengths. In terms of the composition of the seawater solution, beside the (a) (b) principal salt, NaCl, it also contained MgCl2 and MgSO4 magnesium salts, which caused not only a sulphateFigure 14. aggression, (a) SEM image but also of the a magnesium3H0 sample after one. seawater attack; (b) SEM image of the 3H6 sample after seawater attack. Buildings 2020, 10, 67 15 of 18

In the penetration of the composites with ODFA by the solutions containing sulphate ions, a significant role is played by the size of pores and the content of aluminate oxide and . The products of the reaction of magnesium sulphate with calcium hydroxide are, successively, calcium sulphate and hydrate, which in the presence of C3A turn into . Moreover, brucite can also be created. Generally, composites made of cement and FA are characterized by increased resistance to aggressive factors [58]. These properties, together with the increment of the FA content, strengthen the composite. In the case of sulphate aggression, its intensity decreases with the diminishment of C3A[28,59–63]. In spite of the very aggressive environment to which the samples of composites with ODFA, lime and a limited cement quantity were subjected to for 120 days, compressive strength of a minimum of 3 MPa was obtained.

5. Conclusions The results of the research allow us to conclude the following:

1. Large amounts of ODFA and a limited amount of cement were used in composites. The quantity of ODFA was, respectively, 240% and 360% of the cement mass used. Such volumes of this specific kind of FA are not used for the production of cement composites. This problem has also been virtually unaddressed in the research. 2. With the usage of ODFA as a partial replacement of sand (20%–30%), it is possible to obtain the assumed technological properties of cement composites and limit the onerousness of this unwanted waste for the environment to a great degree. This is reasonable, but only with the addition of Ca(OH)2. 3. Composites with additives of different quantities of Ca(OH)2 (2%, 4%, 6%) had considerably higher compressive strength than composites with the same quantity of cement and ODFA but without Ca(OH)2. 4. The samples with ODFA, but without Ca(OH)2, obtained significantly lower compressive strengths (on average by ca. 2 MPa), both before and after the attack, compared to the samples with ODFA and Ca(OH)2. 5. The samples with ODFA and Ca(OH)2 reached the compressive strength of 4.9–6.2 MPa before seawater attack and 3.07–3.85 MPa after it. 6. Although ODFA did not meet the requirements of the PN-EN 450-1 standard pertaining to FA for production of concrete, their presence did not to a higher destruction in aggressive solutions than in composites made from traditional raw materials. 7. Ash concretes are applied in road building and for construction of foundations with compressive strengths from 1.5 to 8 MPa. Composites with ODFA and Ca(OH)2 as an activator can be applied for construction of town district road foundations and bike paths of the compressive strength class C3/4. Moreover, they can be used for foundations subjected to application of de-icing agents. Author Contributions: The individual contribution and responsibilities of the authors were as follows: conceptualization, J.H. and A.R.; methodology, J.H. and A.R.; investigation, J.H. and A.R.; formal analysis, J.H.; writing—original draft preparation, A.R.; writing—review and editing, J.H.; visualization, J.H. and A.R. All authors have read and agreed to the published version of the manuscript. Funding: This research received no external funding. Conflicts of Interest: The authors declare no conflict of interest.

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