Construction and Building Materials 163 (2018) 482–495

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Effect of aggressive chemicals on durability and microstructure

properties of concrete containing crushed new concrete aggregate and
non-traditional supplementary cementitious materials
Mohammed Fouad Alnahhal a, U. Johnson Alengaram a,⇑, Mohd Zamin Jumaat a, Belal Alsubari a,
Mamoun A. Alqedra b, Kim Hung Mo a
a
Centre for Innovative Construction Technology (CICT), Department of Civil Engineering, Faculty of Engineering, University of Malaya, Kuala Lumpur 50603, Malaysia
b
Department of Civil Engineering, Faculty of Engineering, The Islamic University of Gaza, P.O. Box 108, Gaza Strip, Palestine

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

RHA, POFA and POCP were used as

SCMs in concrete made of RA.

The deterioration depth caused by
acid was 2–4 times less for SCMs-
based concrete.

Less propagation of micro-cracks
observed for SCMs-based concrete
attacked by sulfate.

The chemical compositions of
concrete mixture is a significant
factor affecting its performance.

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

Article history: The increasing awareness and usage of traditional supplementary cementitious materials (SCMs) in con-
Received 15 August 2017 crete have pressured the construction industry to look for alternatives to overcome the concerns over
Received in revised form 9 December 2017 their plentiful availability in the future. This research illustrates the performance of recycled aggregate
Accepted 12 December 2017
concrete prepared with the incorporation of available industrial by-products, namely rice husk ash
(RHA), palm oil fuel ash (POFA) and palm oil clinker powder (POCP) as alternatives for traditional
SCMs. The effect of hydrochloric (HCl) acid and magnesium sulfate (MgSO4) attack was evaluated by mea-
Keywords:
suring the change in mass, compressive strength and microstructural analysis. The results revealed that
Concrete durability
Microstructure
the incorporation of RHA, POFA and POCP up to 30% minimizes concrete deterioration and loss in com-
Supplementary cementitious materials pressive strength when the specimens were exposed to HCl solution. In addition, the scanning electron
Acid attack microscopy image showed less propagation of micro-cracks caused by expansive ettringite in the case
Sulfate attack of MgSO4 attack. Further, the X-ray diffraction analysis indicated that RHA is more effective as pozzolanic
additive than POFA and POCP. Overall, the RA-based concrete had significant enhancement in its perfor-
mance against acid and sulfate attacks using alternative SCMs from industrial by-products.
Ó 2017 Elsevier Ltd. All rights reserved.

⇑ Corresponding author.
E-mail address: [email protected] (U.J. Alengaram).

https://doi.org/10.1016/j.conbuildmat.2017.12.106
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 483

1. Introduction This research was conducted with the long-term aim of devel-
oping sustainable and high-quality materials for use as alternative
Durability and versatility of concrete have made it the world’s SCMs. RHA, POFA and POCP were utilized as partial substitution of
most used construction material [1]. Consequently, the use of sup- cement to determine the resistance of concrete made with 100% RA
plementary cementitious materials (SCMs) is becoming more against aggressive chemical attacks. Previous investigations dealt
extensive in the concrete industry due to their potential for with the effect of traditional SCMs, such as fly ash and silica fume
improving long-term properties [2]. Typically, ordinary concrete on the durability properties of RA-based concrete [13,25,26]. In
contains about 10–15% cement and 60–80% aggregate by volume addition, there is limited research on the properties of RA-based
[3]. Taking into consideration a typical concrete mix proportions concrete incorporating POFA [27], and there are no research works
for the 3300 million tonnes of cement and the 22,000 million ton- on the behavior of RA-based concrete containing RHA and POCP
nes of aggregates consumed annually [4], the world produces under chemical attacks. Therefore, the ability of RA-based concrete
11,000 million cubic meters of ready mixed concrete, which makes to withstand the natural aggressive environments was investigated
concrete the largest consumer of natural resources. Recently, the using hydrochloric acid (HCl) and magnesium sulfate (MgSO4)
utilization of recycled concrete aggregate (RA) from construction solutions. Moreover, microanalysis was considered, since the dura-
and demolition waste has attracted the attention of researchers bility properties are related to the microstructure of concrete. The
as a sustainable and feasible material to replace the conventional variables investigated in this research include the percentage of
aggregate in concrete [5]. Nevertheless, there is a consensus by cement replacement by RHA, POFA and POCP (0%, 10%, 20%, and
researchers that the broad use of RA in concrete is hindered by 30%), in addition to the whole replacement of conventional aggre-
its ability to withstand different aggressive environments, such gate by RA. Further, the tests were conducted for a period up to
as water absorbency, chemical attacks and exposure to seawater 120 days, since the use of SCMs is commonly associated with con-
[6,7]. crete properties at later ages.
The relatively higher porosity of RA compared with normal
aggregate makes the RA-based concrete more susceptible to dam-
2. Materials and methods
age when exposed to acid or sulfate solutions. The permeable voids
found in the old mortar adhering on the RA particles allow the 2.1. Materials
entry of acid ions, which in turn degrades the concrete and
decreases its mechanical properties due to chemical reactions 2.1.1. Cement
A commercial ordinary Portland cement (OPC) with strength grade of 42.5 MPa
between acid ions and hydration products [8,9]. Moreover, these conforming to ASTM C150 was used throughout this research.
voids allow the ingress of sulfate ions to the pore structure and
react with the hydration products to form gypsum and ettringite,
2.1.2. Supplementary cementitious materials (SCMs)
which the latter is expansive in nature, leading to the deterioration
Three types of industrial by-products were evaluated for use as SCMs, namely
of the concrete’s surface [6,10]. Hence, the capability of concrete RHA, POFA and POCP. Both POFA and POC collected from palm oil mill were ground
members to resist various aggressive environments is a key dura- using Los Angeles abrasion machine, whilst RHA was purchased from supplier and
bility issue that affects the performance of concrete structures. directly used in the concrete. POFA was collected in the form of ash with relatively
While the RA-based concrete in its beginnings only designed large particles, while large chunks of POC were collected with flaky, porous, and
irregular shapes, and then crushed to smaller sizes. In order to improve the reactiv-
using conventional cement [11], later it was developed using
ity of POFA and POC, they were further ground using a Los Angeles abrasion
blended cement with traditional SCMs including silica fume, fly machine with a speed of about 33 revolution per minute for 30,000 cycles to
ash and ground granulated blast slag to improve its mechanical achieve a sufficient fineness and to match the requirements of ASTM C618. Fig. 1
and durability properties [12,13]. Furthermore, traditional SCMs shows the physical appearance of these SCMs compared with OPC. Their chemical
and physical properties can be found in Table 1. It can be seen that the properties
have been utilized to develop self-consolidating concrete [4], fibre
of RHA, POFA, and POCP conform to the requirements of ASTM C618 for use as
reinforced concrete [14], geopolymer concrete [15] and light- SCMs.
weight concrete [16,17]. Consequently, the practice of using SCMs The scanning electron microscopy (SEM) image of the particle shape and surface
is increasing, where more than 60% of ready-mixed concrete uses texture of OPC, RHA, POFA and POCP are illustrated in Fig. 2. It can be seen that the
SCMs nowadays [18]. While concrete industry is expected to particles of OPC are solid and spherical in some cases. On the other hand, the par-
ticles of RHA, POFA and POCP are irregular. Furthermore, it is obvious from the
expand at a faster rate over time, the current trend involves using
images that the outer surface of the POFA is porous, while the surfaces of RHA
locally available industrial and agricultural waste ashes from the and POCP are made up of sharp edges.
residues of rice and palm oil industries as alternative SCMs [19,20]. The particle size distribution of the binding materials is presented in Fig. 3. It
Rice husk ash (RHA) is about 18–22% by weight of rice husk can be clearly seen from the curves that RHA and POFA have similar fineness of
OPC, while POCP is relatively coarser.
after the combustion process in boilers at temperature of about
800–900 °C in biomass plants. RHA contains over 90% (up to 95%)
amorphous silica, which enhances the pozzolanic reaction in mix- 2.1.3. Aggregates
tures containing Portland cement [21]. Chatveera and Lertwatta- Local mining sand with maximum size of 4.75 mm was used as fine aggregate in
all mixes. Fig. 4 shows the normal aggregate (NA) and RA with a maximum size of
naruk (2011) [22] concluded that the durability of mortar
20 mm that used as coarse aggregates. All aggregates were used at air dried condi-
exposed to acid attack was significantly improved when the tion. The moisture content of sand, NA and RA was 0.87%, 0.15% and 2.36% respec-
cement was partially replaced by RHA, due to the improvement tively. Moreover, the specific gravity, compacted bulk density and water absorption
in the impermeability of the cement matrix. of NA and RA were found as 2.60 and 2.31, 1481 and 1370 kg/m3, and 0.77% and
Pam oil fuel ash (POFA) and palm oil clinker (POC) are by- 4.76%, respectively. Since this research focuses on the effect of SCMs on RA-based
concrete, the RA was extracted from old concrete specimens that has consistent
products produced from different combustion processes of palm characteristics to minimize the potential effect of impurities on the new concrete.
oil residues in a thermal power plant. POFA is the resulting ash In addition, the quality of demolished structures varies in a wide range due to
after the combustion of these residues, and it is about 5% by weight the different compressive strengths of the structures, and hence, the compressive
of the original solids, while POC can be collected as large chunks strength of those old specimens used in this research was known and this would
minimize the number of variables. Therefore, the RA was extracted from old con-
after the burning process. The assessment of pozzolanic activity
crete cubes, cylinders, prisms, and reinforced beams that have been produced using
of POFA and palm oil clinker powder (POCP) confirmed that they conventional materials. The compressive strength, splitting tensile strength, flexu-
are pozzolanic materials, since they have high amount of silica ral strength, and modulus of elasticity of the old (parent) concrete were 51.7, 4.16,
content (>60%) [23,24]. 4.90 and 34120 MPa, respectively.
484 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

Fig. 1. Physical appearance of (a) OPC, (b) RHA, (c) POFA and (d) POCP.

Table 1
Chemical and physical properties of OPC, RHA, POFA and POCP.

Properties OPC RHA POFA POCP ASTM C618 class F

SiO2 (%) 21.0 91 64.17 60.29
Al2O3 (%) 5.9 0.35 3.73 5.83
Fe2O3 (%) 3.4 0.41 6.33 4.71
SiO2 + Al2O3 + Fe2O3 30.30 91.76 74.23 70.83 70 (minimum)
CaO (%) 64.70 0.49 5.80 3.28
SO3 (%) 2.40 1.21 0.74 0.31 5 (maximum)
Loss on Ignition (%) 0.90 4.81 11.56 5.23 12 (maximum)*
Specific gravity 3.14 2.03 2.14 2.53
Retained on 45-mm sieve (%) 13.6 1.70 11.6 29 34 (maximum)
Median particle size (mm) 22.47 19.41 17.62 37.97
*
The use of Class F pozzolan containing up to 12.0% loss on ignition may be approved by the user if either acceptable performance records or laboratory test results are
made available [28].

100
90 OPC
Cumulative Passing (%)

80 RHA
70 POFA
60 POCP
50
40
30
20
10
0
0.01 0.1 1 10 100 1000
Particle Size (µm)

Fig. 3. Particle size distribution of binders.

Fig. 2. SEM image of binders. 2.3. Specimen preparation and testing methods

Steel moulds were used for casting of all concrete specimens and compacted
using a vibrating table. All specimens were kept moist cured from the time of mold-
ing until the moment of test [30].

2.2. Mixtures proportions

2.3.1. Compressive strength
The concrete mix proportions used throughout this study were designed based Concrete cubes of 100 mm were used for the compressive strength test at the
on the Department of Environmental (DOE) method [29] to produce concrete with a ages of 28 and 90 days, in accordance with BS EN 12,390-3.
characteristic compressive strength of 30 MPa. The mix proportions of all concrete
mixes can be found in Table 2. NAC mix was used as control for comparison with 2.3.2. Rate of water absorption (sorptivity)
the RAC mix in which the NA were wholly replaced by RA. The remaining mixes This testing method was intended to determine the susceptibility of concrete to
were produced using 100% RA and incorporated with RHA, POFA and POCP as par- the penetration of water by means of capillary suction (Hall (1989) [31] called the
tial replacement of cement at levels of 10%, 20% and 30%. phenomenon ‘‘water sorptivity”). The test was conducted on specimens measuring
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 485

Fig. 4. The coarse aggregates used in this study (a) crushed granite and (b) recycled concrete.

Table 2
Mix proportions of concretes.

Mix Effective w/b ratio Mix proportions (kg/m3) Slump (mm)

Binders Effective water Mixing water Coarse Fine aggregate SP
aggregate
OPC RHA POFA POCP NA RA
NAC 0.55 380 – – – 209 215 1020 – 750 0.8 140
RAC 0.55 380 – – – 209 232 – 943 750 0.8 125
RHA10 0.55 342 38 – – 209 232 – 943 750 0.8 110
RHA20 0.55 304 76 – – 209 232 – 943 750 0.8 90
RHA30 0.55 266 114 – – 209 232 – 943 750 0.8 80
POFA10 0.55 342 – 38 – 209 232 – 943 750 0.8 120
POFA20 0.55 304 – 76 – 209 232 – 943 750 0.8 115
POFA30 0.55 266 – 114 – 209 232 – 943 750 0.8 80
POCP10 0.55 342 – – 38 209 232 – 943 750 0.8 140
POCP20 0.55 304 – – 76 209 232 – 943 750 0.8 115
POCP30 0.55 266 – – 114 209 232 – 943 750 0.8 95

100-mm Ø  50-mm height at the ages of 28 and 90 days. The test measures the immersion [33]. The solution was replaced every two weeks to maintain a constant
increase in water depth resulting from the absorption of water when only one sur- concentration throughout the test period. Companion specimens cured in water
face of 100-mm diameter is exposed to water. The exposed surface of the specimen were also tested for comparison.
is immersed in water and water ingress of unsaturated concrete is dominated by
capillary suction during contact with water. The measurements were recorded for
2.3.4. Sulfate attack
a period of 8 days, and the correlation between water depth and time is presented.
The sulfate resistance of the concrete was evaluated in this study using the
The sorptivity test was performed according to the guidelines stated in ASTM
method outlined in ASTM C1012 [34]. Concrete cubes of 100-mm were exposed
C1585. The test setup is shown in Fig. 5.
to standard solution containing magnesium sulfate (MgSO4) with about 5% concen-
tration after 28 days of casting. The change in compressive strength was deter-
mined after 28 and 120 days of immersion in the solution and compared with
2.3.3. Acid attack companion specimens cured in water for the same period. Moreover, the solution
The resistance of concrete exposed to acid attack was evaluated in accordance was replaced at regular intervals of two weeks to maintain the pH value between
with ASTM C267 [32] by immersing cubes of 100-mm in 3% hydrochloric acid 6.0 and 8.0 during immersion time.
(HCl) solution after 28 days of casting. Concrete specimens were used to determine
the deterioration depth, mass loss and compressive strength loss after 75 days of
3. Results and discussion

3.1. Compressive strength development

The development of compressive strength of concrete speci-

mens cured in water for a period of 28 and 90 days is shown in
Fig. 6.
It can be observed that the replacement of NA by RA resulted in
a decrease in the compressive strength by about 21%. This could be
due to the large amount of old mortar found in the RA particles
being of an inferior quality compared to the NA, as shown in Fig. 7.
For RA-based concretes containing SCMs, blended mixes with
10% and 20% RHA showed an enhancement in compressive
strength compared with RAC mix, while the contribution of POFA
and POCP to compressive strength was low at the age of 28 days.
On the other hand, Fig. 6 shows that the compressive strength of
concretes containing SCMs has a considerably attainment after
Fig. 5. Set-up of sorptivity test. 90 days of water curing. The compressive strengths of RHA10
486 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

Designed Strength

Fig. 8. ITZ of (a) RA-based concrete and (b) NA-based concrete.

Fig. 6. Compressive strength of concrete specimens at the age of 28 days and 90

days.

(c)
(a) (a)
(b)
(c)
(b) Fig. 9. Zones of weakness in (a) RA-based concrete and (b) NA-based concrete.
(a)
(b) (a)
3.2. Effect of RA on interfacial transition zone of concrete

(c) Sharp edges In order to detect the effect of RA on the interfacial transition
1 cm zone (ITZ) of RA-based concrete, some specimens have been
analyzed by scanning electron microscopy (SEM) image. Fig. 8
(a) (a) illustrates the bond between old cement mortar (represented by
RA particles) and new cement mortar in the ITZ of RA-based con-
Fig. 7. RA-based concrete sample showing examples of: (a) old mortar, (b) stone
crete. In addition, Fig. 8 shows how cement paste is bonding with
particles and (c) new mortar. stone particle in the ITZ of NA-based concrete. It can be observed
that the ITZ in RA-based concrete is more entangled than the one
observed in NA-based concrete, which could be due to the rough
and RHA20 were higher by 20% and 13%, while the strength of surface and the sharp edges of RA particles compared with NA,
RHA30 was slightly lower by 1% than that of the RAC. Moreover, as shown in Fig. 7 [37]. Moreover, it is known that the failure mode
in contrast to the 28-day compressive strength of concrete contain- of Grade 30 concrete due to compression is linked, to a large
ing POFA and POCP, the compressive strength showed an improve- extent, with the quality of aggregate and cement matrix. However,
ment at the age of 90 days. According to these results, it can be the bond between the aggregates and the cement matrix plays an
observed that the compressive strength of RA-based concrete con- effective role in controlling the failure mode. Though the RA used
taining 10–30% RHA, 10–20% POFA and 10–20% POCP is similar or in this research is assumed as strong as the normal aggregate
higher than that of the corresponding RAC mix at the age of 90 (NA), the adhered mortar on the surfaces of RA might fail faster
days. Alnahhal et al. (2017) [2] concluded that the main factor con- than the NA. This can be explained by the fact that the RA has
tributing to the enhancement of compressive strength at the age of rougher surface due to adhered mortar, and hence, the sharp edges
90 days could be the active silica found in RHA, POFA and POCP. existing in RA will generate concentrated stresses, which in turn
This enhancement has been confirmed and discussed using X-ray lead to the failure of the old mortar on the surfaces of RA. On the
diffraction (XRD) and scanning electron microscopy (SEM) analysis other hand, in case of NA-based concrete, the failure is observed
in Section 3.6. The XRD patterns shown in Fig. 21 for the samples to pass through the ITZ, which is considered as the weakest zone
cured in water indicate that the pozzolanic reaction takes place in concrete with Grade 30. This phenomenon is illustrated in
between SiO2 and Ca(OH)2 to form extra C–S–H gel, where the Fig. 9, where the failure is observed to be passed through zones
C–S–H peaks are more prominent and lower intensity peaks of of weakness represented by failure in ITZ in case of NA-based con-
portlandite were observed in samples containing RHA, POFA and crete and failure of the old mortar in case of RA-based concrete.
POCP compared with the control RAC.
The results of this research are in line with those of Tangchira-
pat and Jaturapitakkul (2010) [35] who concluded that concrete 3.3. Sorptivity
containing 10% POFA had a higher compressive strength than
OPC concrete, and the contribution of POFA to compressive The rate of ingress of water or other liquids due to capillary rise
strength increases with increasing curing age. Moreover, Ahmmad is linked, to a large extent, with the penetrability of the pore sys-
et al. (2017) [36] reported that the addition of 15% POCP resulted in tem, which largely affects the performance of concrete subjected
the optimum performance of concrete, and therefore it can be used to aggressive environments. The effect of curing age on the rate
as replacement of OPC. of water absorption of RA-based concrete specimens prepared with
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 487

Fig. 10. The rate of water absorption at the ages of 28 and 90 days.

water absorption was due to the fact that they have high SiO2 con-
tent, thus producing additional C–S–H gel, which the latter has the
potential to fill the existing voids and enhance the resulting pore
structure. Mohammadhosseini et al. (2016) [38] and Islam et al.
(2016) [39] reported that the enhancement against capillary water
absorption of POFA-based concrete is due to the pozzolanic reac-
tion during prolonged curing age, which produced a denser
microstructure, subsequently resulting in a reduction of sorptivity
compared to OPC concrete.

3.4. Effect of hydrochloric (HCl) acid

3.4.1. Acid attack mechanism

The alkaline nature of Portland cement concrete renders it more
susceptible to acid attack [40]. The mechanism of HCl acid attack
can be explained by the progressive neutralization of the alkaline
Fig. 11. Sorptivity values of concrete specimens at the ages of 28 and 90 days.
nature of the cement matrix via the decomposition of hydration
products, e.g. Ca(OH)2 and C–S–H, forming soluble calcium chlo-
ride (CaCl2) salt and water, as explained in Eqs. (1) and (2) [41].
different replacement levels of RHA, POFA, and POCP is illustrated According to Beddoe and Dorner (2005) [42], the pH-stabilities of
in Fig. 10. The sorptivity values in Fig. 11 calculated using the slope Ca(OH)2 and C–S–H found in the deteriorated zones were about
of the line that is the best fit to the points between 0 and 147 s0.5 12.6 and 10.5, respectively. These compounds will be successively
(i.e. 0–6 h). The 28-day sorptivity values of NAC and RAC were decomposed until a silica gel residue is obtained at pH of below 2
0.016 and 0.022 mm/s0.5, respectively. It can be observed that [9], as shown in Fig. 12. Thus, the decalcification of C–S–H could
RAC has sorptivity value higher by about 38% than that of NAC, proceed after the depletion of Ca(OH)2.
which could be attributed to the porous nature of RA compared CaðOHÞ2 þ 2HCl ! CaCl2 þ 2H2 O ð1Þ
with NA, leading to higher rate of water absorption; this has also
been reported by Debieb et al. (2010) [7] for concrete made from C  S  H þ HCl ! CaCl2 þ SiðOHÞ4 þ H2 O ð2Þ
100% of RA.
The 28-day sorptivity values of concretes containing RHA, POFA
and POCP were in ranges of 0.019–0.022, 0.024–0.028 and 0.023– 3.4.2. Decomposition of cement paste
0.030 mm/s0.5, respectively. These results indicate that only the Fig. 12 illustrates the decomposition process of concrete due to
pore structure of RHA-based concrete was improved, since the val- HCl acid attack. The decomposition process yields a tenuous layer,
ues were lower than that of RAC. Moreover, it can be seen that the which progressively increases during the attack [43]. The salient
sorptivity of specimens containing POFA and POCP was higher than observation is the role of the old cement mortar found in the RA
that of RAC, and it increases with increasing replacement level. particles in facilitating the penetration of HCl ions, leading to fur-
However, the sorptivity of concrete specimens containing SCMs ther deterioration in the sound concrete. Hence, the decomposition
showed a significant enhancement after a curing age of 90 days. of cement matrix leads to increase porosity and permeability of the
At this age, the ranges of sorptivity improved to 0.014–0.017, concrete, which in turn causes a reduction in strength and mass.
0.018–0.023 and 0.020–0.023 mm/s0.5 for concretes containing Fig. 13 shows the deteriorated depth of hardened concrete after
RHA, POFA and POCP, respectively, compared with 0.021 mm/s0.5 exposure to 3% HCl solution for a period of 75 days. It can be seen
for RAC. The results showed that the resistance of RA-based con- that the deteriorated depth of RAC is slightly higher than that of
crete against water absorption was enhanced after long curing per- NAC, which could be attributed chemically to the presence of addi-
iod (>28 days) using RHA, POFA and POCP at replacement levels of tional Ca(OH)2 in the old mortar, and physically to the permeable
up to 30%, 20% and 10%, respectively. The improved performance of voids found in the mortar attached on the RA particles, promoting
concrete containing the aforementioned SCMs in terms of resisting a further ingress of acid ions and leading to more increase in poros-
ity. In addition, the results showing that the RA-based concretes
488 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

Fig. 12. Decomposition process summary of concrete due to attack by HCl acid.

Deteriorated
depth

Intact
concrete
NAC RAC RHA10 RHA20 RHA30

POFA10 POFA20 POFA30 POCP10 POCP20 POCP30

Fig. 13. Deteriorated depth of concrete specimens exposed to HCl acid.

containing RHA, POFA and POCP have an improvement in the dete- SCM. Further, RHA-based concrete showed lower mass loss than
riorated layer; it was about 2–4 times less than that of RAC, POFA- and POCP-based concretes, which could be primarily due
depending on the cement replacement level. Moreover, concretes to the high pozzolanic activity of RHA with 91% SiO2 content com-
with 30% replacement level of RHA, POFA and POCP show lower pared with 64% and 60% for POFA and POCP, respectively. Further-
deterioration. Besides, it is well-known that the presence of Ca more, mass loss decreases when the replacement level of the
(OH)2 is low in the cement paste of concrete containing SCMs, cement by RHA, POFA and POCP increases up to 30%. This is mainly
due to its consumption during the pozzolanic reaction [44]. As a attributed to the lower adverse effect of Ca(OH)2, since it will be
result of this, the concretes containing SCMs are less susceptible consumed at a greater range at higher replacement levels. Conse-
to deterioration. However, although the incorporation of SCMs quently, the specimens containing SCMs suffers from minor sur-
has reduced the amount of Ca(OH)2, HCl ions still have the ability face erosion and less corner loss, as shown in Fig. 15. Ranjbar
to react with other calcium compounds in cement paste [22]. et al. (2016) [45] observed a low mass loss and corner deterioration
for concrete containing high amounts of POFA due to the progres-
sive depletion of Ca(OH)2 when POFA content increased. Kannan
3.4.3. Mass loss
and Ganesan (2014) [46] reported that the specimens prepared
The percentage of mass loss due to HCl acid attack on speci-
with up to 30% RHA experienced lower mass loss than those with-
mens made of RA and incorporating RHA, POFA and POCP can be
out RHA after 12 weeks of immersion in 5% HCl solution due to the
found in Fig. 14. Based on the results, it can be inferred that replac-
reduction of capillary pores by the formation of extra C–S–H gel
ing NA with RA further increases the mass loss from 8.4% for NAC
during the pozzolanic reaction.
to 10.3% for RAC. This was due to the high water absorption and
volume of permeable voids of RAC compared to NAC. Moreover,
Nuaklong et al. (2016) [8] pointed out that the presence of Ca 3.4.4. Compressive strength loss
(OH)2 in the old mortar found in RA particles reacts with HCl ions, The compressive strength of concrete specimens exposed to 3%
leading to further loss in mass. The ranges of mass loss for the HCl acid solution and those cured in water for a period of 75 days
specimens incorporating RHA, POFA and POCP were 2.1–3.7%, can be found in Table 3. In addition, Fig. 16 illustrates the
4.7–6.9% and 3.5–5.7%, respectively. It can be seen that the SCM- percentage of loss in compressive strength after exposure to HCl
based concretes yielded lower mass loss than that of RAC without acid. It can be seen that RAC suffered from 67% loss in the compres-
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 489

Table 3
Compressive strength of concrete specimens cured in water and HCl solution.

Mix Compressive strength (MPa)

Cured in water Cured in HCl
NAC 50.7 18.8
RAC 39 12.9
RHA10 49.1 25.5
RHA20 45.1 27.9
RHA30 39.3 26
POFA10 39.7 16.4
POFA20 37.7 18
POFA30 33.6 16.5
POCP10 38.4 18
POCP20 37.6 18.6
POCP30 32.9 16.2

Fig. 14. Mass loss of the specimens after exposure to HCl solution.

sive strength compared to 63% for NAC. The high water absorption
and porosity of RA particles allowed the HCl ions to penetrate
through the concrete, thus resulting in increased dissolution of
Ca(OH)2 and decalcification of C–S–H. In the case of RA-based con-
crete containing RHA, POFA and POCP, the loss in compressive
strength was in the range of 34–59%, depending on the cement
replacement level, which is lower than that of RAC. Moreover,
the loss percentage in the compressive strength was lower, when
the replacement level of cement by SCM increased. For instance,
the lowest compressive strength loss of 34% was recorded for the
mix containing 30% RHA compared to 38% and 48% for the mixes
containing 10% and 20% RHA, respectively. Moreover, the compres-
sive strength loss was 51%, 52% and 59% for mixes prepared with
10%, 20% and 30% POFA, respectively. Furthermore, the incorpora-
tion of 10%, 20% and 30% POCP led to a compressive strength loss of
Fig. 16. Percentage of loss in compressive strength after exposure to HCl acid.
50%, 50% and 53%, respectively. Part of the reason that led to lower
compressive strength loss of RA-based concrete incorporating as a cement replacement, a denser concrete with lower susceptibil-
SCMs is the denser and less porous structure of the cement matrix ity to HCl attack was produced, thus the deterioration process was
as a result of the pozzolanic reaction, which prevents the penetra- reduced.
tion of the HCl ions into the inner part of concrete. Furthermore,
the reduced effect of HCl acid on concretes incorporating RHA,
3.5. Effect of magnesium sulfate (MgSO4)
POFA and POCP is attributed to the limited portlandite content
available for reaction compared to that of RAC. Chatveera and Lert- 3.5.1. Sulfate attack mechanism
wattanaruk (2014) [47] reported a similar concept, where the use Fig. 17 shows the complex and overlapping reactions between
of RHA to replace OPC positively influenced acid resistance due to concrete and MgSO4 solution that disintegrate the sound concrete
the improvement in density and impermeability of the concrete. [48]. The MgSO4 attack mechanism normally starts with the reac-
Alsubari et al. (2016) [33] concluded that when POFA was used tion between hydration products and MgSO4 ions that penetrate by

Fig. 15. (a) Corners and edges deterioration of concrete specimens after exposure to HCl solution, and (b) the attacked specimens after compression test.
490 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

Fig. 17. Possible reactions between concrete and MgSO4 solution.

Table 4
Compressive strength of the specimens cured in water and MgSO4 solution.

Mix Compressive strength (MPa)

28 days 120 days
Cured in water Cured in MgSO4 Cured in water Cured in MgSO4
NAC 47.6 49.8 53.0 48.1
RAC 37.1 39.5 40.2 35.5
RHA10 45.2 45.9 52.0 49.5
RHA20 41.4 42.0 50.8 49.2
RHA30 35.6 35.8 46.5 45.1
POFA10 37.3 38.2 42.9 39.4
POFA20 32.7 33.4 40.3 37.3
POFA30 30.0 30.2 36.5 34.0
POCP10 35.3 35.8 41.7 39.0
POCP20 34.2 34.4 42.2 39.7
POCP30 29.7 30.0 38.3 36.5

absorption property from external sources to form Mg(OH)2, Cured in MgSO4 for 28 days Cured in MgSO4 for 120 days
magnesium silicate hydrate and gypsum (CaSO42H2O), as shown
Relative Compressive Strength

in Eq. (3) and Fig. 17 [49]. The increased concentration of gypsum 1.1 Cured in water
promotes the conversion of tricalcium aluminate (C3A) to ettrin- 1.05
gite, as shown in Eq. (4) [50]. The progressive formation of ettrin-
gite, which is inherently expanding, leads to generate stresses 1
beyond the capability of the tensile strength of the cement matrix
0.95
[51], which in turn causes subsequent cracks and reduction in the
strength [52]. 0.9

MgSO4 þ CaðOHÞ2 þ 2H2 O ! MgðOHÞ2 þ CaSO4 0.85

 2H2 O ðgypsumÞ ð3Þ 0.8

Tricalcium aluminate þ gypsum ! ettringite ð4Þ

Mix Designation

Fig. 18. Relative compressive strength of specimens cured in 5% MgSO4 compared

3.5.2. Effect of sulfate attack on compressive strength
with those cured in water.
The compressive strengths of concrete specimens initially cured
in water for 28 days (zero time) and then immersed in 5% MgSO4
solution for a period of 28 and 120 days are shown in Table 4. It strength of NAC and RAC increased by about 5% and 7%, respec-
can be seen in Fig. 18 that the compressive strength slightly tively, while the increment was in the range of 1–3% for the spec-
increased after 28 days of immersion, then decreased after 120 imens containing SCMs. On the other hand, after 120 days of
days of immersion in MgSO4 solution compared to the specimens immersion, the compressive strength decreased by about 9.2%
cured in water. After 28 days of immersion, the compressive and 11.7% for NAC and RAC, respectively, while for concretes
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 491

Fig. 19. SEM image of concrete specimens cured in (a) water, (b) HCl solution, and (c) MgSO4 solution.

containing RHA, POFA, and POCP, it decreased by about 3.0–4.8%,

6.9–8.2% and 4.7–6.5%, respectively. It is apparent that the incorpo-
ration of RHA, POFA and POCP decreases the negative impact of
MgSO4 solution on concrete. Furthermore, the superficial increase
of compressive strength of the specimens exposed to MgSO4 solu-
tion for a period of 28 days could be attributed to the formation of
ettringite, which leads to a more closed pore structure and slight
increase in compressive strength; the same concept was also
reported by Jo et al. (2017) [53], who stated that the presence of
more voids in the pore structure of cement matrix are able to
30 µm 10 µm
accommodate the expansive ettringite during the early stages of
immersion. Consequently, the continuous formation of ettringite,
that has a relatively large volume, caused internal cracks due to
Fig. 20. SEM image of ettringite needles growing inside the pores of concrete
continuous expansion and resulted in a decrease in the compres- exposed to sulfate solution.
sive strength after 120 days of immersion. A similar phenomenon
was observed by Heikal et al. (2015) [49], when they revealed that
the compressive strength of specimens subjected to aggressive sul- the pore refinement process that occurred as a result of pozzolanic
fate solution increased with curing time up to 90 days, then reaction.
showed a reduction after 120 days of immersion. However, the
decalcification of hydration products can be reduced using SCMs 3.6. Microstructural analysis
due to the pozzolanic reaction, which prevents the diffusion of sul-
fate ions throughout the cement matrix. Limbachiya et al. (2012) The scanning electron microscopy image and X-ray diffraction
[54] pointed out that the inclusion of fly ash in RA-based concrete analysis were performed on concrete samples containing RHA,
would decrease the reactive aluminates (C3A) content, hence POFA and POCP at replacement level of 30% for comparison with
reducing the formation of ettringite. Chindaprasirt et al. (2007) RAC samples. The samples were extracted from concrete exposed
[55] reported a similar observation when using pozzolanic materi- to HCl and MgSO4 solutions, and compared to those cured in water.
als to produce blended cement. They revealed that the use of fly
ash and RHA at replacement level of up to 40% improve resistance 3.6.1. Scanning electron microscopy analysis
against sulfate attack. Tangchirapat et al. (2009) [56] concluded It can be seen from the scanning electron microscopy (SEM)
that the concrete specimens incorporating 10% and 20% POFA images in Fig. 19 that the cement matrix of concretes blended with
had higher compressive strengths than those without POFA, even RHA, POFA and POCP at level of 30% has a uniform and more closed
after soaking in sulfate solution for period up to 180 days, due to microstructure than that of RAC under water curing condition. The
492 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

RAC RHA30

Cured in MgSO4
Cured in MgSO4

Cured in HCl Cured in HCl

Cured in water Cured in water

POFA30 POCP30

Cured in MgSO4
Cured in MgSO4

Cured in HCl Cured in HCl

Cured in water Cured in water

Fig. 21. XRD patterns of RAC, RHA30, POFA30 and POCP30 specimens cured in water as compared with those exposed to HCl and MgSO4 solutions. Peaks labelled with Q:
Quartz, P: Portlandite, C: Calcium Silicate Hydrate, Ct: Calcite, G: Gypsum, E: Ettringite, CC: Calcium Chloride.

Table 5
The main phases detected in specimens cured in water, HCl and MgSO4 solutions.

Phase Peaks at 2H Remarks

Quartz 20.9°, 26.6°, 39.5° and The quartz phase doesn’t reflect one of the hydration products as it might be due to the presence of SiO2 that
SiO2 50.1° can be found in the sand particles.
Portlandite 18.1°, 34.2°, 47.3°, 50.9° Blended concretes with RHA, POFA and POCP showed lower intensity peaks of portlandite than RAC.
Ca(OH)2 and 54.5°
Calcium silicate hydrate 31.92° This peak more prominent in specimens containing RHA, POFA and POCP.
3CaO2SiO24H2O
Calcite 29.4° This peak was greatly reduced after exposure to HCl and MgSO4 solutions.
CaCO3
Calcium chloride 37.1° Due to HCl attack, these peaks were recorded in all samples but with low intensities due to their high
CaCl2 solubility in water.
Tricalcium aluminates 33.2° and 47.7° Due to MgSO4 attack, these peaks were found in very low intensity as expected, due to their conversion to
(C3A) ettringite when reacted with gypsum.
3CaOAl2O3
Gypsum 11.6° Due to MgSO4 attack, these peaks were found in very low intensity as expected, due to their conversion to
CaSO42H2O ettringite when reacted with gypsum.
Ettringite 9.1° and 15.8° Gypsum peaks were more prominent in samples immersed in sulfate solution as a result of the reaction
3CaOAl2O33CaSO432H2O between portlandite and MgSO4.

SEM images also indicate that the microstructure of RAC speci- mens blended with RHA showed the best capability of resisting
mens exposed to HCl acid solution has a tenuous surface texture the propagation of the micro-cracks, even though very few cracks
and considerable amounts of precipitated salts compared with were observed; this enhancement could be attributed to the
concrete specimens blended with RHA, POFA and POCP. In the case improved pore structure of RHA concretes that prevents the
of sulfate attack, the SEM images show the propagation of micro- ingress of sulfate ions, which in turn prohibit the formation of gyp-
cracks in the cement matrix with dissimilar degrees from concrete sum and ettringite. Moreover, the concrete specimens blended
to another, due to the formation of expansive ettringite (a needle- with POFA and POCP showed improvement against micro-cracks
like crystals shown in Fig. 20). Nevertheless, the concrete speci- propagation, but at levels lower than that of RHA concretes.
 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495 493

Table 6
Chemical composition and compressive strength of concretes mixes.

Mix Chemical composition (%) Compressive strength (MPa)

CaO SiO2 Al2O3 Fe2O3 CaO/SiO2 28 days 90 days
NAC 64.7 21.0 5.9 3.4 3.08 45.4 48.3
RAC 64.7 21.0 5.9 3.4 3.08 35.8 38.4
RHA10 58.3 28.0 5.4 3.1 2.08 38.9 46.2
RHA20 51.9 35.0 4.8 2.8 1.48 37.0 43.3
RHA30 45.4 42.0 4.2 2.5 1.08 33.3 38.0
POFA10 58.8 25.3 5.7 3.7 2.32 31.0 39.3
POFA20 52.9 29.6 5.5 4.0 1.79 28.5 36.5
POFA30 47.0 34.0 5.3 4.3 1.39 26.1 32.5
POCP10 58.6 25.0 5.9 3.5 2.35 29.7 37.4
POCP20 52.4 28.9 5.9 3.7 1.82 30.4 36.7
POCP30 46.3 32.8 5.9 3.8 1.41 26.5 32.1

3.6.2. X-ray diffraction analysis

The X-ray diffraction (XRD) test was performed to identify the
main crystalline phases of concrete after exposure to HCl and
MgSO4 solutions, and compare them to those cured in water. The
samples were ground into powder after being extracted from the
surface layer of concretes that showed the best performance
against chemical attacks, i.e. RHA30, POFA30 and POCP30, for com-
parison with RAC. Fig. 21 shows the pattern of the peaks for
selected concretes.
Evidently, all concrete samples cured in water showed similar
peaks with different intensities for the main phases of portlandite,
C–S–H and calcite, irrespective of the type of material used. For
instance, the salient peaks at 2b of 18.1°, 34.2°, 47.3° and 50.9°,
which represent the phase of portlandite [53], are more intense
in the case of RAC, while lower intensity peaks of portlandite were
observed in RHA30, POFA30 and POCP30. The C–S–H peaks are
more prominent in samples of RHA30, POFA30 and POCP30 at
2H of 31.92° [53] as portlandite is used to produce additional
C–S–H during the pozzolanic reaction. The XRD results indicate
that RHA is more effective as pozzolanic additive than POFA and
POCP, where RHA30 showed the lowest trace of portlandite,
Fig. 22. Concrete mixtures in the CaO–Al2O3–SiO2 ternary diagram.
followed by POFA30 and POCP30. It should be noted that the peaks
of quartz could be due to the presence SiO2 in sand particles, and it
does not reflect any of hydration products [45]. at the age of 90 days, even though the replacement level was dif-
In the case of specimens immersed in HCl acid solution, the XRD ferent. Table 6 shows the comparison of the major oxide composi-
results showed peaks of gypsum and calcium chloride at 2H of tions of all mixes. For those containing 10% SCM, i.e. RHA10,
11.6° and 37.1°, respectively. The low intensity peak of calcium POFA10 and POCP10, the ratio of CaO/SiO2 was 2.08, 2.32, and
chloride is due to its high solubility in water. Nevertheless, it can 2.35, respectively. Thus, RHA10 contains less CaO and more SiO2
be seen that the portlandite peaks disappeared from all samples than POFA10 and POCP10, which led to the formation of more
due to the penetration of HCl ions, which decompose the hydration C–S–H, and subsequent higher strength. On the contrary, the addi-
products [57]. tion of more SiO2 by increasing the replacement level by more than
The XRD patterns of the specimens exposed to MgSO4 solution 10%, the CaO content will also decrease, where CaO plays a signif-
show peaks of gypsum and ettringite with different intensities, icant role in the development of compressive strength, especially
depending on the type of material incorporated, due to the reaction at the early age [58]. As a consequence of the surplus SiO2, the
between MgSO4 ions and portlandite. The high intensity peaks of hydration process will be prolonged, which is evident in RHA30
gypsum and ettringite observed in RAC samples indicate a high that contains the maximum content of SiO2 among all mixes, but
possibility of deterioration, while these peaks were hardly detected the CaO/SiO2 ratio of 1.08 was very low, making its compressive
in samples of RHA30, POFA30 and POCP30. Table 5 summarizes the strength lower than that of RHA10 and RHA20.
main phases detected in specimens cured in water, acid and sulfate Fig. 22 represents the layout of all concrete mixtures in
solutions. CaO–SiO2–Al2O3 ternary diagram. Qualitatively, it can be seen that
the incorporation of SiO2-rich SCMs leads to decrease the amount
of portlandite and increase the formation of more C–S–H. Never-
3.7. Chemical composition effect of concrete mixtures
theless, Lothenbach et al. (2011) [44] outlined that at excessive
replacement levels, the pH of the pore solution will drop, reducing
3.7.1. Effect of chemical composition on compressive strength
the solubility of the amorphous silicates and thus slowing the rate
The pozzolanicity and ability of the SCM to consume Ca(OH)2
of reaction.
and form more C–S–H is influenced by different parameters, such
as chemical composition, SiO2 content and particle size of the
SCM [18]. Consequently, the level of reactivity depends on the 3.7.2. Effect of chemical composition on acid attack
replacement ratio of OPC by SCM to attain sufficient strength. For Generally, the chemical composition of hydration products for
instance, mixes RHA30 and POFA10 resulted in similar strength SCM-based concrete with SiO2-rich content is characterized by
494 M.F. Alnahhal et al. / Construction and Building Materials 163 (2018) 482–495

lower calcium content than 100% OPC-based concrete (Table 6 and 5. The SEM images showed that the incorporation of RHA, POFA
Fig. 22). The decomposition of cement matrix attacked by acid is and POCP was able to minimize the deterioration of RA-based
primarily due to the release of calcium from the hydration prod- concrete exposed to MgSO4 solution due to the formation of
ucts and, only at very low pH values, due to the release of alu- dense microstructure that inhibits the ingress of sulfate ions
minium and iron [57]. Bassuoni and Nehdi (2007) [59] revealed and reduces the formation of expansive ettringite, which in turn
that the C–S–H structure with high CaO/SiO2 ratio is more vulner- leads to less propagation of micro-cracks.
able to acid attacks, and on the contrary, the decomposition of C– 6. The XRD results showed that incorporation of SiO2-rich SCMs
S–H with low CaO/SiO2 ratio occurs at slower rate. Additionally, decreased the amount of portlandite and formed more C–S–H.
Chatveera and Lertwattanaruk (2011) [22] concluded that the Moreover, the XRD analysis indicated that RHA is more effective
chemical composition and the CaO/SiO2 ratio in concrete mixture as pozzolanic additive than POFA and POCP, where RHA-based
are important factors for evaluating the effect of acid attacks. Con- samples showed the lowest trace of portlandite.
sequently, the C–S–H that produced with low CaO/SiO2 ratio is less 7. The proportion of chemical compositions in concrete mixture is
susceptible to decompose (release of calcium), since it has a crys- a significant factor affecting the performance of concrete
talline structure with low amounts of calcium. These observations attacked by aggressive chemicals. SCM-based concrete with
also support the results of this study, where the superior perfor- SiO2-rich content is characterized by lower calcium content
mance was recorded for concretes containing low CaO/SiO2 ratios than 100% OPC-based concrete. Thus, the hydration products
(refer to Table 6, Figs. 14 and 16). are less susceptible to decompose (release of calcium) when
exposed to acid. In addition, the content of reactive C3A will
3.7.3. Effect of chemical composition on sulfate attack be reduced, where the latter is considered as reactive com-
The position of concrete mixture on the CaO–Al2O3–SiO2 tern- pound responsible for the formation of ettringite.
ary diagram could be useful to determine its sulfate resistance.
For instance, if the concrete mixture falls within the gehlenite
region as shown in Fig. 22, it typically has a low resistance against
sulfate attacks [60]. This could be related to the high C3A content in Acknowledgement
this region, where C3A is considered as the reactive compound
responsible for ettringite formation. However, the results of this The authors are grateful to University of Malaya for the financial
study showed that the SCM-based concretes have lower CaO con- support through the University of Malaya Research Project-
tent than that of RAC, and thus, the resulting content of reactive RP037A-15AET ‘‘Enhancement of Concrete Properties Made from
C3A will be reduced. Therefore, in this ternary diagram, one would Local Waste Materials Using Nano Particles”.
expect to see a shift of the SCM-based concrete mixtures away
from the gehlenite region. Donatello et al. (2013) [41] revealed that References
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