Construction and Building Materials 143 (2017) 234–246

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Construction and Building Materials

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Toxicity characteristics and durability of concrete containing coal ash as

substitute for cement and river sand
Mahdi Rafieizonooz a,⇑, Mohd Razman Salim b, Jahangir Mirza c, Mohd Warid Hussin d, Salmiati b,⇑,
Rawid Khan e, Elnaz Khankhaje a
a
Faculty of Civil Engineering, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Bahru, Malaysia
b
Center of Environmental Sustainability and Water Security (IPASA), RISE, Universiti Teknologi Malaysia, 81310 Johor Bahru, Malaysia
c
Dept. of Materials Science Research Institute of Hydro-Québec Varennes (Montreal), Québec J3X 1S1, Canada
d
UTM Construction Research Centre (UTM CRC), Faculty of Civil Engineering, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Bahru, Malaysia
e
Department of Civil Engineering, University of Engineering and Technology, Peshawar, Pakistan

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Sustainable concrete produced with

coal bottom ash and fly ash as
Fly Ash Cement
substitute for fine aggregate and OPC, Sulphate Attack

respectively. Blended Cement

Compressive strength, sulfate attack,

Bottom
Sand
acid attack and elevated temperature Ash
effects on the coal ash concrete are Fine Aggregate Age (days)

Change in compressive strength %

determined.
Coal

Pulse velocity, reduction in mass, Water
ơf = 6.6581ơm - 10.94
R² = 0.9288
Coal Fired Power Plant
change in strength and micro- Coarse Aggregate Elevated
structural tests are performed. Temperature
Fabrication of Coal Ash Concrete

TCLP test is performed to analyze the
leaching behavior of BA, FA and coal
Mass loss in %
ash concrete.

a r t i c l e i n f o a b s t r a c t

Article history: The main aim of this study was to investigate the toxicity characteristics and durability of concrete con-
Received 11 December 2016 taining bottom ash (BA) and fly ash (FA), as partial or total replacement of fine aggregate and Ordinary
Received in revised form 3 March 2017 Portland cement (OPC), respectively. Concrete mixtures were prepared containing 0, 20, 50, 75 and
Accepted 16 March 2017
100% of BA as a substitute for river sand and 20% of FA as a replacement for OPC. Tests carried out were
Toxicity Characteristics Leaching Procedure (TCLP), sulfate and acid attack (change in compressive
strength, microstructure and weight) and elevated temperature effects (loss in compressive strength
Keywords:
and mass as well as change in pulse velocity). Results showed that submerging coal ash concrete
Bottom ash
Fly ash
(CAC) mixtures in 5% sulfuric acid solution resulted in less reduction of compressive strength and mass
Toxicity characteristics loss compare to that of the control concrete. Moreover, sulfate resistance tests on concrete mixtures indi-
Coal ash concrete cated that there were no mass loss and no reduction in compressive strength of all the mixtures after sub-
Compressive strength mersion in 5% magnesium sulfate solution. CAC showed higher weight loss and greater compressive
Sulfate attack strength reduction at elevated temperatures. From TCLP results, it is concluded that none of the elements
Sulfuric acid attack leached higher than the maximum concentration of contaminants for toxicity characteristics. It indicates
Elevated temperature that transportation, disposal and utilization of BA and FA as clean construction material’s replacement
could be utilized to reduce their environmental problems, increase efficiency and reduced unit cost pro-
duction of concrete.
Ó 2017 Elsevier Ltd. All rights reserved.

⇑ Corresponding authors.
E-mail addresses: mahdi.rafieizonooz@gmail.com (M. Rafieizonooz), salmiati@utm.my ( Salmiati).

http://dx.doi.org/10.1016/j.conbuildmat.2017.03.151
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246
1. Introduction
At present, concrete is one of the most extensively used materi-
als in construction projects. Most of the materials used in the pro-
duction of concrete are natural aggregates such as river sand and
crushed stone. In Malaysia, natural resources used as fine aggre-
gate are diminishing rapidly. High consumption of natural
resources has led to environmental degradation [1]. Consequently,
decreasing the utilization of these resources as construction mate-
rials through the application of industrial by-products wastes in
manufacturing concrete is a right step towards sustainable devel-
opment [2–5].
Previous researches showed that it is possible to produce dur-
able and sustainable concrete utilizing industrial by-products
waste materials such as red mug aggregates, silica fume, blast fur-
nace slag, coal fly ash (FA) and coal bottom ash (BA), etc. [5–7]. In
Malaysia, generating power results in a staggering production of
BA and FA with rates of 1.7 and 6.8 million tons annually respec-
tively. By the year 2024, it is predicted that Malaysia will have to
rely on coal and gas (58% and 25% respectively) to generate elec-
tricity [8]. Although there are some disparities between the afore-
mentioned figures and those of 2014 (43% coal), it is likely that the
requirement for fossil fuels could increase. This increase in utiliza-
tion of coal will lead to generate of more coal ash that could even-
tually result in more environmental problems.
Several studies have investigated the performance of concrete
incorporating BA as a river sand (fine aggregate) replacement [9–
11]. Accordingly, the microstructure and strength properties of
concrete incorporating BA as replacement of fine aggregate
showed encouraging results [12,13]. Mohammadhosseini et al.
[14] studied the durability performance of concrete incorporating
palm oil fuel ash (POFA) as cement replacement with the addition
of waste carpet fibers. They reported that the effect of POFA on
durability performance of concrete at longer curing periods was
more significant. Hyeok-Jung et al. [15] investigated the effects of
tire derived fuel ash (TDFA) as replacement of cement on the dura-
bility of binder concrete. They reported that concrete containing
TDFA could provide a reasonable improvement in durability due
to packing effect.
The durability performance of concrete containing palm oil
waste materials was studied by Islam et al. [16]. They found that
the increase in POFA by up to 50% gave improved sulfate resistance
of the OPS concrete. Singh and Siddique [13] studied the perfor-
mance of concrete containing BA as sand replacement when
exposed to sulfuric acid attack. According to their study, after
84 days of immersion time, BA concrete containing 100% BA as
replacement of natural river sand, showed 56% reduction in 28 d
compressive strength as compare to 66% reduction for normal con-
crete at the same period of immersion. However, the combination
of utilizing FA as partial replacement of OPC and BA as partial or
total replacement of sand had been studied by only few researches
[7]. The detailed studies concerning the durability of concrete
incorporating BA as sand and FA as OPC substitute are required
before they can be accepted in the production of concrete as con-
struction material.
Moisture movements in concrete are able to cause deterioration
due to the effects of both sulfuric acid and sulfate attack. Concrete
made with BA as fine aggregate replacement have demonstrated
notable performance when subjected to the aforementioned chem-
ical attacks. Singh and Siddique [13] studied the performance of
concrete containing BA as sand replacement when exposed to sul-
fate and sulfuric acid attack. The authors observed that durability
of BA concrete increased slightly compared to that of control con-
crete when subjected to sulfuric acid attack. In addition, they also
found that the resistance characteristics of BA concrete to sulfate
attack were almost similar to that of normal concrete.
235
Elevated temperature is also capable of affecting the perfor-
mance of concrete during its intended lifetime. The main
causes, which influence the heat resistance of concrete, are
temperature and duration of fire, type of cement and aggre-
gates used in its structure, the relative humidity of concrete
and size of structural members. Once the temperature
surpasses 100 °C, the existing water in the concrete will begin
to vaporize and subsequently build up internal pressure inside
the concrete. Excessive internal pressure causes cracks and
spalling of concrete. At temperature of near 500 °C, the calcium
silicate hydrate (C-S-H) in concrete starts to decompose and
dehydrate and at near 900 °C, C-S-H gel will decompose
completely. The compressive strength of concrete decreases
due to C-S-H gel decomposition which then results in the
development of cracks.
BA is a spongy material and its presence as substitute for river
sand in concrete will result in a spongy structure. Concrete with
higher sponginess can be assumed as positive when it is exposed
to high temperature of up to 200 °C. The cause might be due to
the incomplete evaporation of internal water. Yuksel et al. [17]
assessed the effects of high temperature on the performance of
BA concrete and found that by increasing the temperature, residual
compressive strength reduced with increasing in the replacement
ratio.
However, our literature study reveals that some of these wastes
contain heavy metals, which can be leached to the environment.
Therefore, during production process, evaluation of leaching per-
formance of replacement materials is essential. There are several
researches documenting heavy metal concentrations and leachates
in coal ash from different countries such as Australia [18], USA
[19], India [20], South Africa [21], Zimbabwe [22] and Pakistan
[23], etc. The majority of these studies focused on leaching behav-
ior of heavy metals from unbound coal ash. However, their findings
are in contrast with each other: Some researchers [24,25] stated
that some heavy metals could be leached out from coal ash;
whereas others [22,26,27] reported that the leaching of mentioned
elements from coal ash was unimportant. These conflicting find-
ings might be due to differences in leaching method and proce-
dures, variability in type and origin of coal burned, types of
boiler, degree of coal pulverization, firing conditions in the furnace,
ash handling practice and processing technologies used in thermal
power stations.
The objectives of this research were to evaluate the leaching
behavior of BA, FA and crushed concrete particles containing
100% BA as river sand and 20% FA as cement replacement respec-
tively. Furthermore, effects of utilizing BA and FA as partial or total
substitution of fine aggregates and OPC, respectively, on concrete
properties such as toxicity characteristics, compressive strength
and durability were investigated. Durability characteristics of the
concrete were determined using micro-structural analysis with
Scanning Electron Micrographs (SEM) for both sulfate and sulfuric
acid attacks and Ultra Pulse Velocity (UPV) for elevated
temperature.
2. Experimental program
2.1. Materials
2.1.1. Cement
In this research, Ordinary Portland Cement (OPC) used met the
standard requirements of ASTM C150 [28]. Table 1 summarizes its
chemical compositions. In addition, the OPC possessed a blain sur-
face area of 3990 cm2/g, specific gravity of 3.15 and soundness
value of 1.0 mm as well as initial and final setting times of 125
and 210 min, respectively.
236 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246

Table 1
Chemical composition of OPC, FA and BA.

Compound OPC (%) FA (%) BA (%) ASTM C 618 – 15 (%)

SiO2, Silicon dioxide 20.4 47.6 45.3 –
Al2O3, Aluminium oxide 5.20 23.8 18.1 –
Fe2O3, Iron oxide 4.19 7.4 19.84 –
CaO, Calcium oxide 62.39 10.7 8.70 –
MgO, Magnesium oxide 1.55 1.50 0.69 5.0 max
Na2O, Sodium oxide – 2.1 – –
K2O, Potassium oxide 0.005 1.4 2.48 –
TiO2, Titanium oxide – 2.92 3.27 –
P2O5, Phosphorus pentoxide – 1.16 0.351 –
MnO, Manganese oxide – 0.12 0.248 –
SO3, Sulfur trioxide 2.11 0.73 0.3 5.0 max
BaO, Barium oxide – 0.1 0.311 –
LOI Loss on ignition (%) 2.36 0.43 0.1 6.0 max
SiO2 + Al2O3 + Fe2O3 29.79 78.82 83.24 70 min

2.1.2. Fly ash (FA) BA Sand Lower Limit Upper Limit

The FA was obtained from Tanjung Bin coal power plant, located 100
in Johor, Malaysia. It was incorporated as 20% substitution of 90
cement in all coal ash concrete (CAC) mixtures with specific gravity 80

Percent Passing
70
of 2.45, blain surface area of 3450 cm2/g and soundness of 1.0 mm.
60
Table 1 shows its chemical composition. 50
Through FESEM image (Fig. 3), it is shown that in contrast to BA, 40
FA had a regular and spherical shape. It also had smaller particles. 30
As shown in Fig. 1 and through XRD result, Quartz (SiO2), Mullite 20
10
(Al6Si2O13) and iron oxide (Fe2O3) are the main phases present in 0
FA. The sum of SiO2, Al2O3 and Fe2O3 was approximately 78.82%, 0.01 0.1 1 10 100
which can be categorized as Class F in accordance to ASTM C618 Particle Size (mm)
[29].
Fig. 2. Grading curve of BA and Sand.

2.1.3. River sand

The river sand used complies to the description of ASTM C778
[30] and its gradation was in agreement to the requirement of
ASTM C33/C33M [31]. The fine aggregate of river sand was
obtained from Sungai Sayong quarry, Johor (Malaysia). Its physical
characteristics are displayed in Table 2.
2.1.4. Coal bottom ash (BA)
Similar to FA, BA was obtained from Tanjung Bin coal power
plant. Fig. 2 illustrates the particle size distribution of both the
BA and river sand. BA was graded according to the requirements
of ASTM C33/C33 M [31]. Prior to using BA as sand replacement,
it was sieved through a 4.75 mm sieve. Its chemical composition
is summarized in Table 1. The total SiO2, Al2O3 and Fe2O3 in BA
was 83.24%. In addition, the loss on ignition (LOI) value of BA
was around 0.1%. Physical characteristics of BA, sand and coarse
aggregate are shown in Table 2. The particles of BA in contrast to
FA particles are irregular, bigger in size and have rough texture
(Fig. 3). Fig. 1 indicates that Quartz, Mullite, Tridymite syn and iron
oxide are the main phases present in the BA.
2.1.5. Coarse aggregate
The crushed limestone was collected from Bukit Namu quarry,
Johor, Malaysia. Its physical properties are presented in Table 2.
In this research, the maximum size of the coarse aggregate was
20 mm.

Q: Quartz
M: Mullite
I: Iron oxide
Q T: Tridymite syn

M Q I
M Q
I M M
M Q M
a)
Q

M
I M M
M T T M
I M T
b)

Fig. 1. XRD spectrum of FA and BA.

 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246 237

BA FA
Fig. 3. FESEM image of BA and FA.

Table 2 is extensively applied to categorize hazardous solid wastes and

Physical characteristics of BA, sand and coarse aggregate.
Material BA River sand Coarse aggregate
Specific gravity 1.88 2.62 2.69
Water absorption (%) 11.61 7.4 0.61
Fineness modulus 3.44 2.67 6.48
2.2. Concrete mixture Proportioning and casting
Various percentages of BA (0–100%) as fine aggregate and FA
(0–60%) as OPC replacement were used to prepare sixteen batches
of concrete. Based on the compressive strength and workability
results of initial sampling, the concrete mixtures with 20% FA as
OPC substitute and various percentages of BA (25, 50, 75 and
100%) as river sand substitution were selected for further analysis.
In this research, saturated surface dry (SSD) BA and river sand
were utilized. BA was used by mass in concrete as fine aggregate
substitute. In addition, 205 kg/m3 of water was used for all mixes
to obtain a fixed water to cement ratio (w/c) of 0.55. The amount
of cement and slump range were the same for all prepared
concrete mixes, which were 375 kg/m3 and 6–18 cm respectively.
To calculate the mixture propositions (Table 3), the British
method, BS EN 206 [32] was utilized. The components of concrete
were blended in a 0.03 m3 capacity mixer. Concrete cubes of
100 mm  100 mm  100 mm size were cast to evaluate the
compressive strength and durability properties when subjected
to sulfuric acid attack, sulfate attack and elevated temperature.
2.3. Test methods
2.3.1. TCLP
The United States of Environmental Protection Agency (US EPA)
established toxicity characteristic leaching procedure (TCLP). TCLP
estimate the maximum leachate concentration under landfill con-
ditions [33]. 50 g oven dried samples of BA, FA and crushed CAC4
under investigation was weighed and placed in a 2 Liter High Den-
sity Polyethylene (HDPE) bottles. The particle size of the crushed
concrete and BA was kept less than 9.5 mm according to the
requirement of the TCLP procedure [34]. It was then extracted for
18 h with an amount of extraction liquid equal to 20 times (Liquid
to Solid 20:1) the weight of the solid phase.
The extraction liquid employed was chosen based on the waste
alkalinity: Extraction Fluid 1: pH = 4.93 ± 0.05 for sample with ini-
tial pH < 5 and Extraction Fluid 2: pH = 2.88 ± 0.05 for sample with
initial pH > 5. For this study extraction fluid 1 was selected due to
initial pH for materials (BA, FA and CAC4 particles) below 5. Anal-
ysis of the samples was performed in triplicate and the pH of the
filtrate was measured. The leachates were maintained highly acidic
(using nitric acid) to avoid any change in concentration and stored
at 4 °C for metal analysis.
2.3.2. Compressive strength
Based on BS EN 12390-03 [35], the compressive strength was
measured at the intervals of 7, 28, 91 and 180 days of curing. The
cube specimens with SSD condition were exposed to a 3000 kN
compression testing apparatus. Subsequently, a constant load
was applied to all the samples at the rate of 5.0 kN/s. This was done
until the samples could no longer withstand any further additions
load.
2.3.3. Acid resistance
The resistance of concrete cube samples were examined after
being subjected to external sulfuric acid attack [36]. Each concrete
sample was weighed after initial curing period of 28 days in water.
Subsequently, the samples were exposed to 5% sulfuric acid solu-
tion. The changed in compressive strength and mass reduction of

Table 3
Mixture proportion.

Codes Mix proportions (Kg/m3) Slump (mm)

Cement Fine aggregate W (w/c =0.55) Coarse aggregate
FA Cement BA Sand
Control 0 375 0 780 205 1035 73
CAC1 75 300 141 585 205 1035 92
CAC2 75 300 281 390 205 1035 76
CAC3 75 300 422 195 205 1035 53
CAC4 75 300 562 0 205 1035 37
238 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246
the samples were evaluated after 28 d, 91 d and 180 d of submer-
sion period in 5% sulfuric acid solution respectively. The percent-
age loss in mass of each sample after submersion in acid solution
was calculated using Eq. (1):
Winitial  Wt
W ð%Þ ¼  100
Winitial
where W (%) is the percentage mass loss, Winitial is the mass of the
samples before submersion in sulfuric acid solution and Wt is the
mass of the samples at (t) days after submersion in sulfuric acid
solution.
The decrease in compressive strength after submersion in sulfu-
ric acid solution was calculated using Eq. (2):
f cð28 dÞ  f cðtdÞ
f c ð%Þ ¼  100
f cð28 dÞ
where fc is the compressive strength reduction, fc (28 d) represents
28 days compressive strength of the concrete specimens and
fc (t d) is the compressive strength at (t) days after submersion in
sulfuric acid solution.
SEM determined the microstructure analysis of concrete speci-
mens exposed to sulfuric acid solution.
2.3.4. Sulfate resistance
The sulfate resistance of concrete was determined by evaluating
the decrease in compressive strength and weight loss observed in
the concrete mixtures after submersion in 5% magnesium sulfate
solution at different ages. The decrease in compressive strength
and weight of samples were evaluated after 28 d, 91 d and 180 d
of submersion in 5% magnesium sulfate solution respectively.
Compressive strength reduction was calculated using Eq. (2).
SEM was used to determine the microstructure analysis of con-
crete mixtures after being exposed to magnesium sulfate.
2.3.5. Heat resistance
The heat resistance of concrete specimens was evaluated by
heating them in a furnace at temperatures of up to 800 °C. Concrete
cube specimens were prepared as per procedure outlined in com-
pressive strength test and with the same mixing proportion as
shown in Table 3. Prior to testing, three specimens of all concrete
mixtures were weighed, tested for UPV and compressive strength
without any elevated temperature at normal temperature of
27 °C. Subsequently, other concrete specimens were exposed to
temperatures of 200 °C, 400 °C, 600 °C and 800 °C (three specimens
for each temperature for each mixture) at an incremental rate of
4.4 °C per minute. Upon acquiring the desired temperature, the
specimens were placed inside the furnace for approximately 1 h.
The specimens were allowed to cool naturally inside the furnace
at 25 ± 2 °C. Finally, hardened concrete tests were conducted for
the compressive strength and UPV test.
3. Results and discussion
3.1. TCLP
The toxicity of BA, FA and crushed concrete particles of CAC4
mixture (containing 100% BA as sand replacement and 20% FA as
replacement of cement) were analyzed by the Toxicity Characteris-
tic Leaching Procedure (TCLP) test. According to U.S. EPA [34] and
based on initial pH of BA, FA and CAC4 particles, extraction fluid 1
was selected for TCLP method. Table 4 shows the results of TCLP in
comparison with standard regulation. According to this table, all of
the elements showed much lower leaching results than standard
regulation as mentioned by US EPA SW-846. In addition, the con-
centration of heavy metals in CAC4 particles was reduced when
compared to BA and FA. It might be due to encapsulation process
caused by cement paste. From previous studies, it is revealed that
cement paste yields a chemical bonding and physical encapsula-
tion for retaining trace elements including heavy metals effectively
[37].
ð1Þ The results of this research are in agreement with the findings
by [22,27,38]. They also found that the leaching of heavy metals
from coal ash concrete were insignificant and should be ignored.
In fact, disposal, transportation and utilization of BA and FA could
be considered as construction materials in production of sustain-
able concrete. However, long term leaching test as well as pH
dependant leaching test should be carried out for understanding
the leaching behavior of compacted and impermeable material like
concrete.
ð2Þ
3.2. Compressive strength
Fig. 4 illustrates the findings of the compressive strength test.
From the Figure, it is clear that the development of compressive
strength for CAC mixtures upon curing time were almost compara-
ble to that of the control concrete. Additionally, with the increment
of BA content as sand substitute, the compressive strength of CAC
mixtures reduced after 7 d of curing. At the curing time of 7 d, the
compressive strength of mixtures CAC1 (20% FA – 25% BA), CAC2
(20% FA – 50% BA), CAC3 (20% FA – 75% BA) and CAC4 (20% FA –
100% BA) were 9.9%, 18.6%, 22.8% and 25.8% less when compared
to the compressive strength of the control concrete mix, C0,
respectively.
Likewise, at the age of 28 d, all four experimental mixtures
showed lower compressive strength in comparison to the control
concrete. In contrast to the control concrete, the compressive
strength of the experimental CAC mixtures increased at a higher
rate with the increase in the curing age. After 91 d of curing time,
the compressive strength of all mixtures was almost similar to
each other. It could be due to pozzolanic activity of BA and FA
particles.
At the age of 180 d, the compressive strength of CAC mixtures
CAC1, CAC2, CAC3 and CAC4 were 35.9 MPa, 36.0 MPa, 36.6 MPa
and 36.1 MPa respectively. On the contrary, the control concrete
attained 35.9 MPa. It can be concluded that at the curing age of
180 d, all the experimental CAC mixtures exhibited almost identi-
cal compressive strength when compared to the normal control
concrete. This increase in compressive strength of CAC mixtures
can be attributed to pozzolanic activity of BA and FA particles.
The pozzolanic reaction between BA and FA particles and free lime
in concrete leads to the creation of secondary C-S-H gel in CAC
mixtures which is responsible for better mechanical properties
after 180 d of curing time.
The outcomes of this research were comparable to that reported
by [12,39,40]. They similarly found no considerable change in the
compressive strength of concrete incorporating BA as sand
replacement.
3.3. Acid resistance
Sulfuric acid might be produced from either sulfur dioxide pre-
sents in the atmosphere or bacterial processes in the sewerage sys-
tem which attacks the concrete due to the presence of acid. The
formation of sulfuric acid in pipe lines by bacteria results in the
deterioration of concrete sewer pipes. Sulfuric acid reacts with C-
S-H gel in the concrete and forms calcium sulfate. The reaction of
C-S-H gel with sulfuric acid also leads to the production of silicate
oxide (SiO2). The reduction in compressive strength, weight loss
and change in microstructure of CAC samples against submersion
in 5% sulfuric acid solution are discussed. The average of the three
 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246 239

Table 4
BA, FA and CAC4 particles TCLP test result (mg/L).

Materials As Ba Be Cd Cr Co Cu Pb Hg Ni Se Ag Tl V Zn
BA 0.004 0.491 0.005 0.005 0.027 0.002 0.020 0.023 0.047 0.033 0.006 0.073 0.030 0.004 0.196
FA 0.093 0.107 0.019 0.011 0.294 0.008 0.037 0.024 0.000 0.082 0.033 0.028 0.008 0.000 0.047
CAC4 0.000 0.426 0.002 0.001 0.015 0.009 0.000 0.011 0.000 0.014 0.001 0.006 0.002 0.000 0.021
Standard Limitation 5.00 100.00 0.75 1.00 5.00 80.00 25.00 5.00 0.20 20.00 1.00 5.00 7.00 24.00 250.00

Control CAC1 CAC2 CAC3 CAC4 decomposition of C-S-H gel. Furthermore, the mixtures experi-
40 enced loss of cement paste and sample size reduction.
Upon 180 days of submersion, the percentage reduction in
Compressive Strength (MPa)

35
30
25
20
15
10
5
0
0 50 100
Age (days)
Fig. 4. Change in compressive strength with time for control and CAC mixtures.
samples taken from the same mixture was used to evaluate the
reduction in compressive strength and mass loss.
3.3.1. Compressive strength reduction
Fig. 5 presents the development of the compressive strength of
all concrete mixtures after submersion in 5% sulfuric acid solution.
Compressive strength of CAC mixtures CAC1, CAC2, CAC3 and CAC4
decreased by 29.22%, 27.11%, 27.83% and 27.21% respectively after
28 days of submersion period, as compared to 35.82% reduction in
the control concrete mixture, C0. In fact, after 28 days of submer-
sion, the compressive strength of CAC mixture CAC3 incorporating
75% BA and control concrete mix, C0, decreased from 25.0 MPa to
18.0 MPa and 31.0 MPa to 19.9 MPa respectively.
After 91 days of submersion period, the values of the 28-day
compressive strength of all concrete mixtures showed a decrease.
Reduction values in the 28-day compressive strength of concrete
mixtures C0, CAC1, CAC2, CAC3 and CAC4 were 47.03%, 40.66%,
39.77%, 36.23% and 36.72% respectively. The decrease is due to sul-
furic acid affecting the concrete matrix to weaken and led to
strength for CAC mixtures CAC1, CAC2, CAC3 and CAC4 were
47.83%, 46.96%, 40.86% and 41.68% respectively as compared to
52.68% reduction in the 28-day compressive strength control con-
crete. The percentage reduction of 28-day compressive strength of
CAC mixtures decreased with the increase in BA content as fine
aggregate replacement. These observations may be due to the
lower permeability of CAC samples, which subsequently improved
the resistance to the external sulfuric acid attack.
150 200
3.3.2. Microstructure
SEM image of concrete mixtures CAC1, CAC2, CAC3 and CAC4
after 180 days submersion in 5% sulfuric acid solution are shown
in Fig. 6. The SEM images indicated that all CAC mixtures became
more permeable upon submersion for up to 180 days. In general,
as the sulfuric acid attack progresses, the C-S-H gel decalcifies
and therefore the Ca/Si molar ratio decreases. Moreover, because
of the loss of cement paste, the specimen’s size is reduced. As
shown in Fig. 6, the permeability decreased by increasing the con-
tent of BA in CAC. It could be due to creation of extra C-S-H gel by
pozzolanic reaction between BA and FA particles with free lime in
concrete. This demonstrated that concrete containing higher per-
centage of BA as replacement of river sand would exhibit better
performance against sulfuric acid attack than that of the normal
concrete.
3.3.3. Loss in weight
Fig. 7 represents the percentage of mass loss in concrete speci-
mens after submersion in 5% sulfuric acid solution for up to
180 days. Generally, CAC mixtures showed slightly better perfor-
mance than the control mixture after the said submersion time.
Following 28 days of submersion, loss in mass of CAC mixtures
CAC1, CAC2, CAC3 and CAC4 were 10.44%, 10.66%, 10.35% and
10.39% respectively as compared to 10.62% that of the control

C0 CAC1 CAC2 CAC3 CAC4

25
Compressive strength (MPa)

20

15

10

0
28 91 180
Age (days)

Fig. 5. Compressive strength reduction after submersion in sulfuric acid solution.

240 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246

CAC1 CAC2

CAC3 CAC4
Fig. 6. SEM of concrete mixtures CAC1, CAC2, CAC3 and CAC4 after 180 days submersion in sulfuric acid solution.

C0 CAC1 CAC2 CAC3 CAC4

16
14
12
Mass loss in % age

10
8
6
4
2
0
7 14 28 60 91 180
Age (days)

Fig. 7. Influence of BA and FA on resistance of concrete to the external sulfuric acid attack (mass reduction).

mixture, C0. The mass loss of CAC specimens reduced with the
increase in BA content in CAC. It might be due to more water is
withhold with BA particles.
At 91 days of submersion period, loss in weight of CAC mixtures
CAC1, CAC2, CAC3 and CAC4 increased to 12.66%, 12.61%, 12.11%
and 12.39% respectively. Similarly, the loss in weight of control
mix, C0, during the same period increased to 12.78%.
Next, at 180 days of submersion, concrete mixtures CAC1, CAC2,
CAC3 and CAC4 recorded mass loss as high as 13.25%, 13.11%,
12.71% and 12.94% as compared to 13.41% for the control mix,
C0. It is believed that by increasing the BA content in concrete
and due to the pozzolanic properties of both BA and FA, the perme-
ability of CAC reduced, unlike the normal concrete. The lower per-
meability of CAC resulted in lower percentage of loss weight in the

CAC specimens in comparison to that of the normal concrete
specimen.
3.3.4. Relation between reduction in compressive strength and
percentage of weight loss (acid resistance)
Fig. 8 represents the relation between the weight loss of
concrete specimens and their decrease in compressive strength
against the submersion in 5% sulfuric acid solutions. The higher
value of coefficient of determination, R2, demonstrated that
there was a good relation between the regression trend and
data points. The mass loss increased almost linearly with the
reduction in compressive strength of the concrete samples.
The relation between the reduction in compressive strength
and weight loss could be due to sulfuric acid submersion and
is given by:
f ¼ 1:5687m þ 35:183 R2 ¼ 0:8605 ðauthorÞ
Singh and Siddique [13] reported virtually similar relationship
between the two variables, which was given by:
f ¼ 4:2383m þ 7:21 R2 ¼ 0:9467
[13] where ơf is the percentage of compressive strength loss and ơm
is the percentage of loss in weight.
The percentage reduction of CAC specimens’ compressive
strength following 28 days was approximately 1.57 times the
percentage of weight loss. This is in accordance with the linear
regression line, obtained in current research.
3.4. Sulfate resistance
Sulfate attack can cause changes in microstructure, mass loss
and alteration in compressive strength in concrete. One of the
most important factors in protecting the concrete against external
sulfate exposure is the permeability of concrete. Given that the
exposure to magnesium sulfate has more intense effect on con-
crete, all concrete samples were subjected to 5% of magnesium
sulfate solution. In extensive diversity of resources such as under-
ground water, soil with high levels of clay, storm water, sea water
and mines, sulfate ions could be found [41]. The effects of sulfate
on concrete are ascribed to the expansion of gypsum and ettrin-
gite. The sulfate ions intrude into the concrete and react with
portlandite Ca(OH)2 to generate ettringite and gypsum. The
ettringite then absorbs moisture to produce expansion and thus
causes expansion which leads to cracking and spalling in concrete
structure [42,43].
22
Compressive strength (MPa)
20
18
16
f = -1.5687 m + 35.183
14
R² = 0.8605
12
10
8 10
Mass loss in %
Fig. 8. Relationship between reduction in compressive strength and weight loss
after 180 days submersion in 5% sulfuric acid solution.
M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246 241
3.4.1. Changes in compressive strength
The increment in compressive strength of all concrete speci-
mens following the submersion in 5% magnesium sulfate solution
was compared to their obtained 28-days compressive strength, as
shown in Fig. 9. After 91 days period of immersion, the increase in
the 28-days compressive strength of CAC mixtures CAC1, CAC2,
CAC3 and CAC4 were 22.35%, 24.64%, 24.39% and 23.38% respec-
tively as compared to 21.44% increase for the control concrete mix-
ture, C0.
Upon 180 days period of immersion, the increase in the 28-days
compressive strength of all concrete mixtures C0, CAC1, CAC2,
CAC3 and CAC4 were 25.18%, 27.67%, 29.81%, 31.99%, and 30.66%
respectively. The increment in the strength of CAC after submer-
sion in 5% magnesium sulfate solution might be due to the contin-
uous hydration of cement paste and the filling of voids with extra
C-S-H gel formed due to the pozzolanic action of both BA and FA.
The confined voids within the formation of ettringites could be
the reason that there was no reduction in compressive strength
and mass loss. The formation of ettringites in voids and continued
hydration of concrete mixtures disrupted the connectivity of pores,
which caused the higher decrease in concrete mixtures’ permeabil-
ity. Due to the reduction in connectivity of pores in the concrete
specimens, the penetration of sulfate ions reduced. Moreover, the
increase in durability of CAC mixtures subjected to sulfate attack
could be due to the lower permeability of CAC mixtures than con-
trol mix. Singh and Siddique [13] found that the compressive
strength of the concrete incorporating BA as a substitute for river
sand increased over their 28-days compressive strength after
180 days of submersion in 10% magnesium sulfate solution. Simi-
larly, Irassar et al. [44] indicated that the compressive strength of
concrete specimen incorporating 40% FA as a substitute of cement
showed an increase of 86% compared to its 28-day compressive
strength after an submersion period of one year.
3.4.2. Microstructure
The deterioration of hardened concrete due to creation of
ettringite and gypsum undergoes a process, which results in the
decrease in both strength and stiffness. The first step of ettringite
formation is also known as the gypsum formation, which can be
identified as the main reason of deterioration of concrete upon
exposure to sulfate attack. SEM images of CAC mixtures CAC1,
CAC2, CAC3 and CAC4 after 180 days of submersion period in 5%
magnesium sulfate solution are shown in Fig. 10. It can be seen
that there were no considerable creation of any new distinct
phases. Actually, Fig. 10 illustrated that no sulfate ion diffusion
existed on or near to surface of the specimens. Indeed, no monosul-
fate morphologies and gypsum were detected in all the specimens
to demonstrate the effects of sulfate attack. Additionally, all the
SEM images showed spread and dense C-S-H gel.
3.4.3. Mass loss
No spalling and cracks were detected in all the specimens dur-
ing the entire period of experiment. Furthermore, no weight loss in
all the mixtures was detected, even after 180 days of submersion in
5% magnesium sulfate solution. The results of this study is compa-
rable to that stated by Singh and Siddique [13]. In their research,
the authors observed no loss in mass in their specimens after
210 days of submersion in 10% magnesium sulfate solution.
3.5. Heat resistance
The most important factors, which influence the resistance of
12 14 16
concrete to the elevated temperature, are the types of cement
and aggregate used and their mixing ratio, moisture content of
the concrete, size of the structural member as well as the temper-
ature and duration of fire. During the heating progression, certain
242 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246

C0 CAC1 CAC2 CAC3 CAC4

35

Change in compressive strength %

30

25

20

15

10

0
28 91 180
Age (days)

Fig. 9. Alteration in compressive strength after submersion in magnesium sulfate solution.

CAC1 CAC2

CAC3 CAC4
Fig. 10. SEM images of concrete mixtures CAC1, CAC2, CAC3 and CAC4 after 180 d submersion in magnesium sulfate solution.

transformations may arise such as chemical decomposition, mois-
ture evaporation and internal vapor pressure. During the early
stages of the heating process, transformations may not be suffi-
cient to cause any cracks.
The presence of water in the concrete will only begin to vapor-
ize when the temperature surpasses 100 °C and subsequently,
building up internal pressure inside the concrete. The excessive
internal pressure then leads to few spalling and cracks of concrete.
At a temperature of approximately 500 °C, the C-H-S gel in the con-
crete begins to dehydrate and decompose and at approximately
900 °C, the C-H-S gel decomposes completely.
Fig. 11 shows the development of cracks in the CAC3 mixture
surface when subjected to elevated temperature. It is clear that
by increasing the temperature, the number, size and depth of
cracks increased. The compressive strength of the concrete is thus
reduced because of the dehydration of C–S–H gel and cracks
development.
3.5.1. Effects on compressive strength
Table 5 displays the effects on compressive strength of the con-
crete mixtures when subjected to elevated temperatures. Consid-
ering the results of residual compressive strength achieved at
 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246 243

200 ° C 400 C
°

a b

° °
600 C 800 C

c d
Fig. 11. Development of cracks in surface texture of CAC3 specimen when subjected to different elevated temperatures.

different temperatures, the evaluation of temperature effects was
based on three temperature zones, namely, zone A, B and C with
temperature ranges of 27–200 °C (zone A), 200–400 °C (zone B)
and 400–800 °C (zone C).
The residual compressive strength of all concrete specimens
decreased gradually with the increase in temperature in zone A
but at a quicker rate within zone B. On the other hand, a sudden
reduction was observed in zone C. The decrease in compressive
strength in zones A and B could be ascribed to the steady dehydra-
tion and decomposition of the cement paste, therefore changing
the physical properties of the concrete from SSD condition to a
dry condition. While in zone C, the sudden reduction in residual
compressive strength detected may be caused by the complete
decomposition of calcium hydroxides and partial dehydration of
C-H-S gel, which occurred at a temperature of over 450 °C.
Fig. 12 represents the decrease in compressive strength of both
normal and CAC mixtures when exposed to elevated temperature
of up to 800 °C. It is seen that in zone A, the CAC showed better per-
formance than the control concrete. However, in the zones B and C,
the control concrete performed better in contrast to all the CAC
mixtures. This may be due to the complete dehydration and
decomposition of extra C-H-S gel in the CACs. Also by increasing
the BA content, the compressive strength of CAC mixtures
decreased. It could be attributed to the fact that more water was
withheld by BA particles thus, more evaporation and internal pres-
sure existed in CAC mixtures. Eventually it results in more reduc-
tion in compressive strength with increased disruption in
concrete matrix and cement paste.
3.5.2. Mass loss
The influence of high temperature on the mass reduction of
both normal and CAC are shown in Fig. 13. Test data revealed that
mass loss occurred in both control concrete and CAC specimens
due to the exposure to elevated temperatures. In addition, mass
loss increased with the rising of temperature. This was expressed
as a percentage of original weight (weight before heating) between
room temperature (27 °C) and mass when subjected to a targeted
temperature.

Table 5
Effects of elevated temperatures on compressive strength of concrete.

Change in compressive strength (MPa)

Mix Normal 91 d Temperature ° C
200 400 600 800
C0 34.48 31.41 26.67 18.12 6.64
CAC1 33.44 29.41 22.44 15.88 4.27
CAC2 34.55 31.72 22.94 16.94 5.31
CAC3 34.20 33.14 28.06 17.49 5.02
CAC4 33.85 32.85 28.14 17.99 4.62
244 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246

Control CAC1 CAC2 CAC3 CAC4

16

14

12

Mass loss in %
10

0
200 400 600 800
Temperature °C

Fig. 12. Reduction in compressive strength when subjected to elevated temperatures.

Mass loss observed in all zones was a result of evaporation of 100

Change in Compressive strength in %

moisture from the concrete surface to the environment [45]. The 90
loss in mass of concrete when subjected to elevated temperature
80
might be ascribed to the changes in mechanical properties and
stiffness of the concrete. The structure of the concrete deteriorates 70 f = 6.6581 m - 10.94
as confirmed by the high weight reduction with the increase in 60 R² = 0.9288
temperature. Owing to the fact that the evaporation of water in 50
C-S-H formation and disintegration of Ca(OH)2, the binding proper- 40
ties of the cement paste is lost [13,46]. CAC showed higher loss in 30
weight when exposed to higher temperature. This might be due to
20
the greater moisture content withheld by BA and FA particles.
Moreover, the loss in weight escalated with the increase of BA con- 10
tent in CAC. 0
0 2 4 6 8 10 12 14 16
3.5.3. Relation between compressive strength loss and mass reduction Mass loss in %
(heat resistance)
Fig. 14. Relation between reduction in compressive strength and mass loss.
Fig. 14 shows the relation between compressive strength loss
and mass reduction of all concrete mixtures due to exposure at ele-
vated temperature. The higher R2 value demonstrated that there is
a good relation amongst the regression trend and data points. The
where ơf represents the percentage of compressive strength loss
reduction in compressive strength due to elevated temperature
and ơm signifies the reduction in weight in percentage.
almost increased linearly with increase in weight loss of the con-
According to the linear regression line that was achieved in this
crete mixtures. The following equation presents the relationship
research, the percentage reduction in the compressive strength of
between both variables when exposed to a high temperature:
CAC mixtures at 91 days was almost 6.65 times the percentage of
f ¼ 6:6581m  10:94R2 ¼ 0:9288 loss in their weight.

Control CAC1 CAC2 CAC3 CAC4

Change in Compressive strength in %

100
90
80
70
60
50
40
30
20
10
0
200 400 600 800
Temperature °C

Fig. 13. Effect of BA and FA on resistance of concrete to elevated temperature (mass loss).
 M. Rafieizonooz et al. / Construction and Building Materials 143 (2017) 234–246
Table 6
UPV of concrete specimens exposed to high temperatures.
Ultra Pulse Velocity (UPV)
Mix Normal 91 d
C0 4313
CAC1 4218
CAC2 4263
CAC3 4339
CAC4 4301
3.5.4. UPV of concrete mixtures subjected to elevated temperatures
Table 6 illustrates the concrete deterioration through Ultrasonic
Pulse Velocity (UPV) measurements performed at selected temper-
atures. Initially the changes in UPV values were low, but with the
increase in temperature, the UPV values reduced drastically. The
UPV values of C0, CAC1, CAC2, CAC3 and CAC4 mixtures at initial
temperature were 4313 m/s, 4218 m/s, 4263 m/s, 4339 m/s and
4301 m/s respectively. However, the values in the range of 3610–
3816 m/s were obtained for all concrete mixtures at a temperature
of 200 °C. This indicated that all concrete mixtures were of good
quality. However, at temperatures between 400 °C and 800 °C,
the results obtained were believed to be doubtful in terms of qual-
ity [47].
The deterioration of the microstructure in the concrete mix-
tures resulted in the reduction of UPV values. Topçu and Canbaz
[46] attributed the said form of changes to the decomposition of
C-S-H gel at a temperature of over 450 °C, which results in the
increase in the pores volume and air voids in the structure of
concrete. Hence, the speed of sound waves transmission is reduced
through the concrete samples, which increases the time required
for ultrasonic pulse to be transmitted.
4. Conclusions
The leaching behaviors of BA, FA and CAC4 particles as well as
effects of the external chemical attack and high temperature on
the concrete properties incorporating both BA and FA as replace-
ment of sand and OPC respectively were studied. The following
conclusions can be drawn from this study:
1. Based on the data obtained from TCLP test, it can be concluded
that none of the elements leached higher than the maximum
concentration of contaminants for toxicity characteristics. It
indicates that transportation, disposal and utilization of BA
and FA as sand and OPC replacement are beneficial to reduce
their environmental problems as well as increase efficiency
and reduce unit cost production of concrete.
2. The performance of CAC in relation to the compressive strength
at similar curing period was comparable to that of the control
concrete. At the early age of curing of up to 28 d the compres-
sive strength of control concrete was higher than that of the
CAC specimens. But as the curing age increased, so did the com-
pressive strength of the CAC specimens. At 91 d curing age, the
compressive strength of CAC specimens was approximately
close to the normal concrete and after 180 d, it exceeded the fig-
ures obtained by the control concrete.
3. In terms of the effects of sulfuric acid attack, CAC mixtures
behaved slightly better than normal concrete. The compressive
strength reduction and loss in mass of CAC mixtures upon sub-
mersion in 5% sulfuric acid solution was less in contrast to the
normal concrete. Accordingly, the decreased in 28-days com-
pressive strength reduced as much as 52.68% for the normal
concrete and only 40.86% for the CAC mixture, which contained
245
Temperature ° C
200 400 600 800
3816 2513 574 438
3745 2617 520 263
3610 2487 537 305
3731 2462 561 467
3773 2427 568 471
75% BA as fine aggregate replacement and 20% FA as cement
replacement upon 180 days.
4. The study on the sulfate resistance of concrete indicated better
changes in compressive strength of CAC specimens in compar-
ison to the normal concrete. Moreover, no weight loss in all
the mixtures was detected even after 180 d period of submer-
sion in 5% magnesium sulfate solution. These results might be
due to the continuous hydration of the cement paste and filling
of voids with extra C-S-H gel formed, as a result of pozzolanic
action of both BA and FA.
5. The CAC mixtures demonstrated higher loss in weight when
exposed to higher temperature rate. This might be because of
larger content of moisture withheld by both the BA and FA par-
ticles. Reduction in mass due to elevated temperatures
increased with the increase in BA content of CAC specimens.
The CAC mixtures performed better than the control concrete
in the first zone. Conversely, the control concrete showed better
performance than all the CAC mixtures in the second and third
zones. This was probably due to the complete decomposition
and dehydration of extra C-H-S gel in the CAC mixtures. Finally,
the results of UPV test showed that at temperature rates of
between 400 °C and 800 °C, the performance and quality of all
concrete mixtures were believed to be doubtful.
Acknowledgement
The authors thank to Universiti Teknologi Malaysia for the
financial support provided through the Ministry of Education
Malaysia under OTR grant, Vot. R.J1300000.7301.4B145. They also
appreciate the support given by the Japan International Coopera-
tion Agency (JICA) under the scheme of SATREPS Program (Science
and Technology Research Partnership for Sustainable Develop-
ment) for the project Development of Low Carbon Society Scenar-
ios for Asian Region.
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