Construction and Building Materials 155 (2017) 296–306

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Construction and Building Materials

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

Mechanical strength and durability properties of concrete containing

treated recycled concrete aggregates under different curing conditions
Sallehan Ismail a,⇑, Wai Hoe Kwan b, Mahyuddin Ramli c
a
Faculty of Architecture, Planning & Surveying, Universiti Teknologi MARA, Perak Branch, Seri Iskandar Campus, 32610 Seri Iskandar, Perak, Malaysia
b
Department of Construction Management, Faculty of Engineering and Green Technology, Universiti Tunku Abdul Rahman, 31900 Kampar, Perak, Malaysia
c
School of Housing, Building and Planning, Universiti Sains Malaysia, 11800 Pulau Pinang, Malaysia

h i g h l i g h t s

The mechanical strength and durability of RAC with treated RCA was studied.

Three different curing regimes were applied.

Sea water remarkably deteriorates the compressive strength of RAC.

Permeability and porosity of specimens are affected by curing regimes.

Use of treated RCA significantly minimize the adverse effects in RAC.

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

Article history: This paper examines the mechanical and durability properties of concrete incorporated with treated recy-
Received 13 April 2017 cled concrete aggregate (RCA) under different curing conditions. Three different curing regimes were
Received in revised form 27 July 2017 applied, namely, continuous normal water curing (NW), initial water curing for 28 days before exposure
Accepted 15 August 2017
to an open air environment (OA), and initial water curing for 28 days before exposure to seawater (SW).
Two concrete mixes were produced by replacing 60% of the coarse aggregate using treated and untreated
RCA with one control specimen (100% natural coarse aggregate) to examine the mechanical strength
Keywords:
(compressive and flexural strength) and durability (water absorption, oxygen permeability, and also
Curing
Durability
porosity) properties of the concrete. Meanwhile, the microstructure of these mixes was studied via scan-
Mechanical strength ning electron microscopy (SEM). The inclusion of untreated RCA generally reduces the mechanical
Recycled concrete aggregate strength and durability of the concrete regardless of the curing conditions. The compressive strength
Recycled aggregate concrete of the concrete containing untreated RCA is more detrimental in SW than in the other two curing condi-
Surface treatment tions. Moreover, the concrete with RCA have poor intrinsic air permeability and porosity because their
intrinsic porosity and effect are more significant when the curing is performed in OA than in the other
curing conditions. Incorporating the treated RCA helps limit the reduction in the mechanical strength
and durability of the concrete particularly under a prolonged curing period.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction
In conventional construction, external curing for concrete is
applied after mixing, placing, and finishing. The main purpose of
curing is to control the fast hydration process of concrete by keep-
ing favourable moist conditions under a suitable temperature [1].
Proper curing of concrete structures is important to ensure that
they meet their intended strength performance and to control
⇑ Corresponding author.
E-mail addresses: salleh_itm@yahoo.com (S. Ismail), kwanwh@utar.edu.my
(W.H. Kwan).
the early volume change. These are related to durability enhance-
ment. In other words, curing will enable the concrete to hydrate
properly with good microstructure development, with less poros-
ity, and with proper strength to maintain concrete dimensional
stability without creeping or shrinkage [1]. On the other hand,
carelessness in curing, particularly at an early stage, can cause
irreparable loss as the concrete will not achieve the desired prop-
erties because of a lower degree of hydration [2]. This can also
cause an early-age crack because of the damaging effects that dry-
ing and possibly autogenous shrinkage create, especially for con-
crete with lower water/cement (w/c) ratios [3].

http://dx.doi.org/10.1016/j.conbuildmat.2017.08.076
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306
The problem of using recycled concrete aggregate (RCA) lies in
the attached residual mortar, which makes RCA characteristically
lower strength, porous and highly absorbent. When RCA is incor-
porated in new concrete to produce recycled aggregate concrete
(RAC), the higher water absorption capacity of RCA causes difficul-
ties in controlling the effective water/cement (w/c) ratio, which
decreases the workability of fresh concrete [4] and consequently
influences the strength [5,6] and durability [7,8] of the hardened
concrete. Moreover effect from high water absorption of RCA and
the use of high total w/c ratio of RAC induce water transfer during
and after hydration. Therefore, the curing conditions have a consid-
erable effect on the final performance of concrete [9]. However the
effect of curing process on RAC depends on the types of curing
regime or condition. Otsuki et al. [10] observed that curing condi-
tions under high relative humidity of up to 90% lead to better
mechanical properties at the ITZ, which can be attributed to the
reduction in the porosity of the ITZ. Buyle-Bodin and Hadjieva-
Zaharieva [9] founded that initial absorption, air permeability
and carbonation depth of RA concrete cured in water is lower than
that was achieved under air storage curing condition. Qi et al. [11]
investigated the effect RAC when exposed to sodium sulfate solu-
tion under wetting-drying cycles for about 9 months and they
observed that the damage of RAC against sulphate attack are signif-
icantly affected by increasing the quantity of RCA replacement.
Research conducted by Chakradhara Rao et al. [12] revealed that
partial curing (combination of wet and dry) condition of RAC effec-
tively and significantly improves the strength compared with cur-
ing in continuous wet condition due to improvements in the old
ITZ. Specifically, in this experimental study, the concrete cured in
air after 7 days of wet curing was observed to show better strength
than concrete cured completely under water for 28 days for all
coarse aggregate replacement ratios. Poon et al. [13] observed that
the compressive strength and modulus elasticity of RAC seem to
exhibit increase in early stage of steam curing period which is
not the case with standard water curing. The steam curing method
was also observed to improve the drying shrinkage and the resis-
tance to chloride-ion penetration. However, the effect of this cur-
ing method is significantly influenced and affected by the
increase of RCA content. In another study, Gonzalez-Corominas
et al. [14] found that the effect steam curing is beneficial to com-
pensate the reduction in long term compressive strength of RAC
made from medium-low quality RCA in comparison with normal
aggregate concrete mixtures. Moreover steam-cured RACs up to
90 days had greater reductions of capillary pores volume thus
results RAC low porosity than natural aggregate concrete. Fer-
nando et al. [15] found that the 28-day compressive strengths of
RAC were found similar to the natural aggregate concrete when
exposed under the standard curing condition while the compres-
sive strength of RAC decrease up to the 20% when they were expo-
sure in open-air conditions. Meanwhile research study conducted
by Fonseca, et al. [16] found that compressive strength results of
RAC seem negligible to be affected by curing conditions or in
another words insensitive to curing condition.
However the effect of higher porosity and water absorption
capacity of RCA has potential to become internal curing agent.
Kim and Bentz [17] reported that blending of RCA and saturated
lightweight fine aggregates provides an internal source of water
to offset the chemical shrinkage that occurs during hydration of
the paste, thus effectively resisting autogenous shrinkage while
maintaining compressive strength reduction. The high absorption
characteristic of RCA which absorbs more water during mixing
results in acting as a natural moisture reservoir to assist in the later
hydration [18]. This reservoir promotes in the formation of calcium
silicate hydrate in the later age and refines the interfacial transition
zone [19], thus would improving the RAC performance. Using sat-
urated or semi-saturated RCA in the concrete positively affected
297
the durability via internal curing. The duration of the curing period
also influences the performance of RAC. The durability of RAC has
been benefited from extended periods of curing [8,9,20]. In addi-
tion, long-term curing period shows that after 5 years, concrete
made with 100% crushed concrete aggregate has the lowest poros-
ity and slightly significant effect in increasing the compressive and
splitting tensile strengths [21].
This research was performed in consideration of our previous
studies [22] on the effectiveness of multi-phase surface treatment
methods in enhancing the properties of coarse RCA. The main aim
of this research is to assess the influence of different types of cur-
ing conditions on the short- and long-term mechanical strength
(compressive and flexural strength) and durability (water absorp-
tion, intrinsic air permeability, total porosity, chloride resistance
and SEM examination) of modified RAC with treated RCA. All test
specimens were subjected to initial water curing for 28 days and
were then exposed to three curing conditions, namely, normal
water (NW), outer/open air environment (OA), and seawater
(SW). The mechanical strength and durability of the modified
RAC were analyzed and compared with those of normal aggregate
concrete and unmodified RAC specimens to determine their
effectiveness.
2. Experimental program
ASTM Type 1 Ordinary Portland cement with a specific gravity of 3.15 g/cm3
was used as the main binder for the experiment (see Table 1 for detail chemical
composition). In this study, all of the coarse aggregates used had a maximum size
of 20 mm. The natural coarse aggregate used was crushed granite. The coarse
RCA used were generated from waste concrete cubes collected from the debris area
and crushed by jaw crushers and then sieve to get the specified size. Two types of
coarse RCA were produced in this study, treated and untreated. The treated RCA is
prepared by modifying the RCA surface structure through the combination of two
different surface treatment methods. In this process, the RCA is initially treated
by soaking in hydrochloric (HCl) acid at 0.5 M (M) concentration for 24 h. They
are then impregnated with wollastonite (calcium metasilicate) solution. The chem-
ical composition of wollastonite is presented in Table 1. The details on the proce-
dures involved in this treatment process and beneficial effect of this surface
treatment were described in previous research [22]. Table 2 provides a comparison
of the properties of coarse natural aggregate (granite) and coarse treated and
untreated RCA in terms of physical and mechanical strength characteristics. Natural
river sand which consisted of particles that passed through a sieve size of 5.00 mm
was used as fine aggregate. Table 3 shows the sieve analysis of the fine and coarse
aggregates that were used in this study, which were graded according to BS 812-
Part 103.1. Other properties of the natural fine aggregates are presented in Table 4.
To enhance the workability of the concrete in this study, chloride-free super plasti-
cising admixture based on sulphonated naphthalene polymers was used during the
mixing of concrete. The physical and chemical properties of the superplasticiser
was formulated in accordance with ASTM C494.
The designated concrete mix proportions were based on a constant effective
water/cement ratio of 0.41 for all concrete mixtures in accordance with the British
method published by the Department of Environment [23] to achieve a target
slump range of 30–60 mm and a compressive strength of 50 MPa on 28 day. Three
series of mixtures were prepared depending on the type of coarse aggregate con-
tent, as follows: (i) specimen type CO (control concrete) was prepared using only
natural coarse aggregates; (ii) specimen types RO refer to RAC composed of
untreated coarse RCA: (iii) specimen types TR refer to RAC composed of treated
coarse RCA. The dosage compositions of the coarse aggregates in this experiment
were kept constant by replacing the natural coarse aggregate with untreated or
treated RCA at 60% of the weight of the total coarse aggregate content in all RAC
mixtures. The detailed mix design and proportions in the constituent materials
for the overall concrete specimens are presented in Table 5.
All concrete mixes in this study were mixed in accordance to the sequence pre-
scribed in BS1881-125 [24]. The specimens were demolded at 24 h after casting,
and then were initially cured under water curing at an atmospheric temperature
of 25 ± 2 °C for 28 days before further exposure to different curing regimes; NW-
series, OA-series and SW-series environments. The NW series are using standard
moist or the specimens were continuously cured in normal water. For the OA series
were placed the specimens in the open area of a laboratory corridor to be exposed
to a tropical climate, which included solar radiation and rain. The ambient temper-
ature ranged from 26 + 2 °C (rainy day) to 35 + 2 °C (sunny day) and the relative
humidity ranged from 60% to 90%. The rationale for this curing was the need to
examine the characteristics of the specimens when subjected to uncontrolled con-
ditions of humidity and temperature, which involved different weathering cycles
such as wetting and drying conditions. Meanwhile the SW series the specimens
298 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306

Table 1
Chemical composition of cement and wollastonite.

Material Chemical composition (%) LOI Specific Gravity (g/cm3)

SiO2 Al2O3 Fe2O3 CaO MgO K2O P2O5 MnO TiO2 Others
Cement 16 3.6 2.9 72 1.5 0.34 0.06 0.03 0.17 3.41 0.64 3.15
Wollastonite 50.32 0.77 0.33 44.44 1.31 0.15 0.08 0.05 0.03 2.52 0.46 2.87

Table 2
Properties of coarse aggregate [22].

Properties of aggregate Sizes of Natural Untreated RCA Treated RCA

aggregate aggregate
After acid soaking After impregnation with
wollastonite solution
% Mortar Content 20 mm 22
10 mm 45
% Mortar loss 20 mm 2.6
10 mm 2.9
Flakiness (%) Random 11 15
Elongation (%) Random 11 19
Particle density, oven dry (Mg/m3) 20 mm 2.60 2.33 2.39 2.39
10 mm 2.58 2.23 2.32 2.34
3
Particle density, saturated surface dry (Mg/m ) 20 mm 2.62 2.43 2.48 2.48
10 mm 2.60 2.35 2.43 2.45
Apparent particle density (Mg/m3) 20 mm 2.65 2.59 2.61 2.61
10 mm 2.63 2.54 2.59 2.61
Water absorption (%) 20 mm 0.60 4.44 3.58 3.48
10 mm 0.70 5.58 4.65 4.48
Bulk density (kg/m3) Random 1507 1292 1313 1348
Agg. crushing value (%) 14 mm 24.32 29.15 28.34
Agg. impact value (%) 14 mm 13.98 21.78 19.26
LA abrasion value (%) 14 mm 34.76 39.12 36.76

Table 3
Sieve analysis of aggregates.

Types of aggregate Aggregate passing (%) according to sieve size (mm) Fine modulus
0.15 0.3 0.6 1.18 2.36 5 10 14 20
Fine Agg. 0.9 8.8 22.7 45.3 77.4 100 100 100 100 3.45
Coarse Agg.
Natural 0.0 0.0 0.0 0.0 0.2 0.2 23.2 59.2 100 6.17
RCA 0.0 0.0 0.0 0.0 0.4 0.8 30 60.4 100 6.08

Table 4 Table 6
Properties of fine natural aggregates. Major ions in sea water.

Properties Value No. Ion Name Amount mg/L

3
Particle density, oven dry (Mg/m ) 2.60 1. Fluoride 3142.33
Particle density, saturated surface dry (Mg/m3) 2.63 2. Chloride 2.88
Apparent particle density (Mg/m3) 2.67 3. Bromide 0.16
Water absorption (%) 1.08 4. Nitrate 2.08
Moisture content 0.31 5. Sulphate 203.02
Fineness 75 mm (%) 0.93

were continuously immersed in sea water. Then, they were stored in a PVC tank
filled with sea water obtained from the seaside along Penang Island. The sea water
was refresh every two months. The major ions in the sea water were analysed via
ion chromatography test and the results are reported in Table 6. All of the speci-
mens were cured in accordance with the aforementioned regimes until the expo-
sure period of specimens reached the testing age of 3, 6 and 10 months.
In this study, the effects of the results of mechanical strength and durability
properties of modified RAC mix specimens were analyzed and compared with the
corresponding to normal aggregate concrete (CO) and also with unmodified RAC
specimens (RO) to determine their effectiveness. The parameters such as compres-
sive strength, flexural strength, water absorption, air permeability and porosity of
hardened concretes were examined at the age of 7, 28, 90, 180 and 300 days. Com-
pressive and flexural strength tests were performed in accordance with BS EN

Table 5
Details of mixing proportion.

Specimen Cement kg/m3 Water kg/m3 Coarse aggregate kg/m3 Sand kg/m3 SP (%)
Gravel RCA
CO 512 210 956 – 722 0
RO 512 210 382 574 722 0
TR 512 210 382 574 722 0.2
 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306 299

12390-3 [25] and BS EN 12390-5 [26], respectively. Water absorption test was con- 70
ducted in accordance with procedures prescribed in BS 1881-122 [27]. The test
specimens consisted of three concrete cylinders with 75 mm diameter and 65

Compressive Strength (MPa)

100 mm height, cored from a representative of each sample of concrete prism.
Intrinsic air permeability of the concrete mixes were determined using a Leeds cell 60
permeameter proposed by Cabrera and Lynsdale [28]. The samples used in the test
consisted of six cylindrical concrete specimens with dimensions of 45 mm 55
Ø  40 mm were obtained by coring from the prisms of each concrete mixture.
CO
The porosity of concrete was determined using the vacuum saturation method 50
developed by RILEM [29]. The same set of specimens prepared for intrinsic air per- RO
meability was used in test as well. The porosity value of each concrete sample can 45 TR
be calculated using the following equation:

msat  mdry 40
P¼  100 ð1Þ
msat  mwater
35
where P is the porosity (%), msat is the weight in air of the saturated sample, mwater is
the weight in water of the saturated sample and mdry is the weight of the oven-dried 30
sample. Chloride penetration test was conducted in accordance with BS 1881–124 0 30 60 90 120 150 180 210 240 270 300 330
[30]. Chloride content was determined using thiocyanate standard solution titrated Curing Age (days)
against 0.1 M silver nitrate. The extraction of the samples from the specimens is
illustrated in Fig. 1. The 25 mm diameter cylinders were cored from the prisms Fig. 2. Compressive strength of tested specimens at NW curing versus curing age.
and then cut into slices according to their respective depth levels. The top 5 mm
from both ends was eliminated. The slices were then ground into extremely fine
powder. The chloride content, J (percentage to mass of cement) was calculated using 70
the following expression:

Compressive Strength (MPa)

  65
V6 m 0:3545 100 CO
J¼ V5   ð2Þ 60
0:1 Mc C1

where, V5 is the volume (ml) of 0.1 M silver nitrate solution added; V6 is the volume 55
(ml) of thiocyanate solution used; Mc is the mass (g) of sample used; m is the molar- RO
50
ity (mol/l) of the thiocyanate solution; and C1 is the cement content (%) of the sample
used. Meanwhile scanning electron microscopy (SEM) analysis were used to 45
strengthen the arguments provided in discussions. The SEM of samples were anal-
ysed under a Quanta FEG 650 microscope. The samples for the SEM profile were 40
TR
obtained from cored specimens from the concrete prism, which were carefully cut,
35
polished, dried and coated with gold.
30
0 30 60 90 120 150 180 210 240 270 300 330
3. Results and discussion Curing Age (days)

3.1. Compressive strength Fig. 3. Compressive strength of tested specimens at OA curing versus curing age.

The results (Figs. 2–4) generally show that all the concrete spec-
imens have similar profile of strength development regardless of 65
the effect of the types of curing conditions, and the compressive
60
Compressive Strength (MPa)

strength increases with the curing period. However, the exposure

to SW appears to deteriorate the compressive strength perfor- 55
mance, and degradation is observed to be greater in unmodified
CO
RAC specimens (RO). A similar finding is reported by Yue, Tan, 50
and Guo [31]. They found that SW remarkably deteriorates the RO

compressive strength of RAC in the marine environment. This dis- 45 TR

crepancy may possibly occur because of SW corrosion due to var-

40
ious salt contaminants (i.e., sodium sulfate, magnesium sulfate,
and chloride) led to the interruption of the hydration of cement 35
and deterioration of the formation structure in concrete, thus low-
ering their strength [31–33]. Islam et al. [33] explained the effect of 30
0 30 60 90 120 150 180 210 240 270 300 330
Curing Age (days)
125 mm 125 mm 125 mm 125 mm
Fig. 4. Compressive strength of tested specimens at SW curing versus curing age.

SW can transform the hydration cement product in lead to increase

100 mm
the secondary formation of expansive products, such as ettringite
and some leachable compound. Meanwhile, the presence of high
magnesium sulfate contaminant in SW would decompose the
CASAH gels in the cement paste with formation of non-
5mm from the cementing magnesium silicate hydrate [34,35]. However, in this
both ends are case, the deterioration in the compressive strength of RAC can be
compensated by using treated RCA. Changing the specimens from
discard
the initial curing condition of fully submerging them in water at
a prolonged period of 28 days and then taking them outside the
Fig. 1. Method of sampling for the chloride penetration test. curing tank to be exposed to ambient (OA) conditions benefits
300 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306

cement hydration. As a result, most of the compressive strength of 8

all specimens cured in this condition is found to be slightly favor-

Flexural Strength (MPa)

able than those prolonged in water during the entire testing per- CO
7
iod. This could be explained as due to the higher curing
temperature, such as that in tropical climates, accelerate the rate
6
of cement hydration [36]. Additionally, when specimens are RO
exposed to an outdoor environment, subsequently their moisture
content is removed. This behavior leads to the release of the dis- 5

joining pressure, and the bonds at the cement matrix structure

4 TR
are strengthened, thus, the compressive strength of concrete is
enhanced [37].
3
0 30 60 90 120 150 180 210 240 270 300 330
3.2. Flexural strength
Curing Age (days)
The effects of curing conditions and flexural strength of all con- Fig. 6. Flexural strength of tested specimens at OA curing versus curing age.
crete mixtures are depicted in Figs. 5–7. An effect can be observed
when specimens are continuously cured in NW, and a similar
reduction trend for the compressive strength is observed when 8
the untreated RCA is incorporated in concrete (Fig. 5). However,
the drop in flexural strength is slightly lower than the compressive

Flexural Strength (MPa)

7 CO
strength. The flexural strength also appears to be less affected
when exposed to other curing conditions (OA and SW). This result
seem contradicts with that of the compressive strength. This pos- 6
sible factor might be caused by the influence of the enhancement RO
at the cement paste–aggregate bond. On the basis of previous
5
results, RCA has angular shape and rough texture compared with
the coarse natural aggregate and might lead to better adhesion
bond and interlocking between the cement paste and the RCA par- 4 TR
ticles compared with those of the natural aggregate [4,38,39].
Additionally, the bond strength between aggregate and matrix 3
highly plays an important role in flexural strength loads [40,41]. 0 30 60 90 120 150 180 210 240 270 300 330
This fact is confirmed when the treated RCA is added in RAC, as Curing Age (days)
indicated in TR specimens, which leads to the improvement of
the flexural strength. The flexural strength of the TR specimens Fig. 7. Flexural strength of tested specimens at SW curing versus curing age.
becomes comparable with that of the CO concrete at different cur-
ing exposures and ages. This result is possibly caused by the avail-
pore networks to create ‘‘wedging effects” [42]. Ramli [43] and
ability of additional binder in the presence of wollastonite coated
Ramli, Kwan and Abas [34] reported that the crystallization of salt
at RCA, which reacts with cement during the hydration process
formation would close and refill within the microstructure of con-
and enhances the interface bond between paste and aggregate.
crete, thus increasing the bonding strength between materials. This
Analysis on the flexural strength performance of all specimens
trend is a primary function that is related to the testing mechanism
that are subjected to three types of curing conditions shows that
of nature, where bonding strength within the matrix of concrete
all specimens significantly benefit from their exposure to SW con-
plays an important role in dealing with flexural tests.
dition, regardless of types of mix and proportions of concrete. Fig. 7
shows that the flexural strength in majority of the specimens cured
in SW is remarkably higher than those specimens cured in other
3.3. Water absorption
curing regimes at different testing ages. The high gain in flexural
strength attained in specimens that are exposed to SW conditions
In general, Figs. 8–10 show that water absorption of all speci-
is caused by the high formation of crystallization of salt within
mens tends to decrease over the curing period regardless of curing
conditions because of the increasing of cement hydration products
8

4.50
Flexural Strength (MPa)

7 CO
4.00
Water Absorpon (%)

CO
6 3.50
RO
5 3.00 RO

2.50
4 TR
2.00 TR

3 1.50
0 30 60 90 120 150 180 210 240 270 300 330 0 30 60 90 120 150 180 210 240 270 300 330
Curing Age (days) Curing Age (days)

Fig. 5. Flexural strength of tested specimens at NW curing versus curing age. Fig. 8. Water absorption of tested specimens at NW curing versus curing age.
 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306 301

4.50

Instrinsic Air Permeability, K ( x 10-16 m2 )

1.20

4.00 1.00
Water Absorpon (%)

3.50 0.80
CO

3.00 RO 0.60 CO

TR RO
2.50 0.40 TR

2.00 0.20

1.50 0.00
0 30 60 90 120 150 180 210 240 270 300 330 0 30 60 90 120 150 180 210 240 270 300 330
Curing Age (days) Curing Age (days)

Fig. 9. Water absorption of tested specimens at OA curing versus curing age. Fig. 11. Intrinsic air permeability of the tested specimens at NW curing versus
curing age.

4.50
1.20

Instrinsic Air Permeability, K ( x 10-16 m2 )

4.00
Water Absorpon (%)

1.00
3.50
0.80
3.00 CO
CO
RO 0.60
RO
2.50 TR
TR
0.40
2.00
0.20
1.50
0 30 60 90 120 150 180 210 240 270 300 330 0.00
Curing Age (days) 0 30 60 90 120 150 180 210 240 270 300 330
Curing Age (days)
Fig. 10. Water absorption of tested specimens at SW curing versus curing age.
Fig. 12. Intrinsic air permeability of the tested specimens at OA curing versus
curing age.
that fill the capillary pores of the cement matrix. However, the flow
absorption rate of specimens may differ among mixes because it
determines the porosity of concrete, whereas the pores inside the 1.20
Instrinsic Air Permeability, K ( x 10-16 m2 )

concrete are determined by material composition and mix

1.00
proportion.
The computed water absorption rate of RO specimens relative
0.80
to the control for all curing conditions and testing ages falls
between 10% and 35%. The influence of porous materials leads to 0.60 CO
a higher water absorption rate; RCA with old cement paste tends RO
to absorb more water [44–47]. The use of treated RCA effectively 0.40 TR
decreases the water absorption rate. This finding is supported by
the water absorption rate obtained from TR specimens for all test- 0.20
ing ages and curing conditions that were relatively lower than
those of RO specimens and closer to the control concrete. The 0.00
0 30 60 90 120 150 180 210 240 270 300 330
low absorption rate of TR specimens can be explained by the
Curing Age (days)
reduced porosity of RCA after surface treatment. In addition, wol-
lastonite particles on the outer surface of the RCA act as fillers in Fig. 13. Intrinsic air permeability of the tested specimens at SW curing versus
reinforcing cementitious materials to produce strong and high curing age.
packing density that is able to refine the capillary void in concrete
structures, thus decreasing the permeability of concrete [48].
thereby causing high permeability, that is, gases and fluids pass
through the concrete structure easily [20,42].
3.4. Intrinsic air permeability In comparing overall concrete mixture, the differences of the
intrinsic permeability values of some RAC specimens become mar-
Figs. 11–13 show the various intrinsic air permeability rates of ginally close to that of the control concrete after 28 days of initial
all specimens cured up to 300 days in NW, OA, and SW conditions. curing. However, after 300 days, the percentage differences in
At 7 and 28 days of initial curing, the lowest permeability rate with intrinsic air permeability rate indicated by RO specimens were still
respect to testing age was obtained by the control concrete. In con- considerably higher than values from the control concrete. The air
trast, all RAC specimens with the inclusion of RCA exhibited higher permeability of RO specimens for a testing age of 300 days is 38%,
intrinsic air permeability than control concrete. The incorporation 96%, and 19% higher than the specimens cured under NW, OA, and
of RCA increased the number of pores in the concrete structure, SW conditions, respectively, than the control specimen. These
302 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306

results suggest that aside from the divergence of hydration forma- 16.0
tion inside the concrete layer caused by the different curing condi-
15.0
tions, the cracks and pores in untreated RAC are considered the
main factors of the increased permeability of concrete. 14.0
The intrinsic permeability of TR specimens was significantly
13.0

Porosity (%)
lower than the effect on RO specimens, especially in the later
age. At a curing age of 300 days, the intrinsic air permeability value 12.0 CO

of TR specimens cured under NW and SW was comparable with the RO

11.0
values from control specimens. TR specimens cured under OA had TR
a 57% higher intrinsic air permeability value than control. How- 10.0
ever, the obtained value was still lower than values from RO spec- 9.0
imens, because the wollastonite particles are able to modify and
refine the pore structure, thereby creating a dense microstructure 8.0
0 30 60 90 120 150 180 210 240 270 300 330
especially at the interface zone between the aggregate and cement
Curing Age (Days)
matrix.
Although the permeability of all mixes decreased with the Fig. 15. Total porosity of the tested specimens at OA curing versus curing age.
increasing age of curing regardless of curing exposure, the intrinsic
air permeability value benefited the most for concrete specimens
cured under prolonged NW and SW environment. Specimens in 16.0
NW and SW conditions have a lower rate compared with speci-
mens exposed to OA. This result is attributed to the uniform and 15.0

good development of cement hydration products, which resulted 14.0

in the availability of enough water supply sources to completely fill
and reduce the porosity in hydrated cement matrix [49]. In addi- Porosity (%) 13.0
CO
tion, the effect of prolonged SW curing may reduce the total poros- 12.0 RO
ity of concrete specimens and the probability of pores being either TR
11.0
blocked or narrowed down by the crystallization of salt [34,50].
Exposure to dry and wet cycles during tropical climate may induce 10.0
expansion and contraction and lead to the initial formation of
9.0
microcracks [34,51], which increase the permeability of concrete.
Exposure to dry conditions can jeopardize the development of a 8.0
0 30 60 90 120 150 180 210 240 270 300 330
dense microstructure because of the absence of water [36].
Curing Age (Days)

Fig. 16. Total porosity of the tested specimens at SW curing versus curing age.
3.5. Porosity

Variations in porosities of all concrete specimens with respect

to testing age and curing conditions are presented in Figs. 14–16.
In general, the obtained total porosity rate of all concrete mixtures
follows a similar trend as the rate gain of intrinsic air permeability,
where the gain in porosity values of all concrete mixtures gradu-
ally decreases with the increase in curing period regardless of cur-
ing exposure because of the continued formation of hydration
products over time, which refines the capillary pores and voids
of the cement matrix (Neville 1995).
For all testing ages, higher porosity were obtained from RO
specimens regardless of curing exposure. For instance, the porosity
of RO specimens was 15%, 17%, and 12% greater than that of control
16.0
15.0
14.0
Porosity (%)
specimens subjected to NW, OA, and SW conditions, respectively.
Due to the greater porosity of untreated RCA, it served as a conduit
for water transport [7,42]. However, the use of treated RCA can
decrease the porosity values of RAC. In certain cases, the change
of exposure from initial water curing to SW curing increased the
porosity of TR specimens with an age of 90 days. However, the
overall gain in the porosity of TR specimens is remarkably lower
than RO specimens in a prolonged curing period. The total porosity
of TR specimens at a testing age of 300 days was only 6%, 5%, and
4% higher than that of control specimens subjected to NW, OA,
and SW conditions, respectively. This finding means that the
improved porosity of TR specimens compared with RO specimens
is associated with the decreased porosity of RCA as a result of sur-
face treatment. Furthermore, the increase in cement hydration for-
mation on the outer layer of RCA particles due to the reaction
between wollastonite particle and cement paste can refine the
pores and densify the microstructure in RAC, thus decreasing its
porosity.

13.0
CO The effects of different curing exposure conditions on the poros-
12.0 RO ity of all specimens are negligible, and the permeability of all mixes
decreased with increasing curing time. The porosity values of all
11.0 TR
specimens in their concrete mixtures and similar testing age under
10.0 their respective curing conditions are comparable with each other.
9.0
However, the effect of continued cement hydration as well as the
increase of salt crystal formation proportional to the increase of
8.0 exposure time can reduce the porosity of all RAC specimens
0 30 60 90 120 150 180 210 240 270 300 330
Curing Age (Days) exposed to SW curing. Thus, the porosity in most RAC specimens,
exposed to SW curing is generally lower than other similar mixes
Fig. 14. Total porosity of the tested specimens at NW curing versus curing age. exposed to different curing conditions.
 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306 303

3.6. Chloride penetration

In this study, chloride profiling test was conducted on all spec-
imens subjected to prolonged immersion in SW conditions. The
chloride profiling testing was also conducted for same specimens
exposed to continuous NW conditions. However, the test was per-
formed only once at the age of 90 days in order to counter check
the effect of surface treatment of RCA relative to the concentration
level of chloride in RAC specimens. Based on the previous section
on aggregate testing, certain levels of chloride were identified in
treated RCA. Additionally, the obtained results can be compared
with specimens exposed to SW conditions. The diffusion of chlo-
ride concentration is determined in each layer of concrete and
expressed as a percentage of the weight of cement. Table 7 show
the variation results of the chloride penetration of all specimens
with respect to curing conditions at testing ages of 90, 180, and
300 days.
In most cases, the specimens in the seawater curing condition
had a high concentration of chloride compared with those in the
normal water condition. The penetration of chloride for all speci-
mens exposed to seawater curing for the entire testing age had
similar profile trends. Chloride concentration was higher at the
first layer (0–10 mm) and gradually decreased as the sampling
depth increased toward the concrete prisms. However, the concen-
tration of chloride at all layers of concrete under SW tended to
increase when exposed to prolonged curing times.
The porosity of the untreated RAC could still be seen as the main
factor that exerts a dominant influence on the RAC and affects the
resistance to chloride penetration when immersed in seawater.
The penetration depth of the chloride ions in unmodified RAC
shown by the RO results was greater than that of the control con-
crete for all testing ages. This finding corresponds to those of pre-
vious studies [7,20,52,53], in which the ingress of the chloride ions
is strongly governed by their permeability on water absorption and
porosity characteristic.
In contrast, using treated RAC had a significant effect in terms of
enhancing the resistance to chloride diffusion. The improvement in
the decreased chloride permeability rate as demonstrated by the
TR specimen may be attributed to the inclusion of treated RCA
decreases the pore structure of concrete.
3.7. Microstructure of the concrete
A fractured concrete specimen is used to identify the
microstructure morphology of aggregate-cement matrix interfacial
zone (ITZ). In Fig. 17, SEM observed small pore structures in the ITZ
between the natural coarse aggregate and cement paste of the con-
Cement paste
Aggregate
Fig. 17. SEM micrograph of ITZ between natural coarse aggregate and cement paste
of control specimen at 28 days.
trol concrete at 28 days, with widths between 500 and 800 nm. The
strong interface bond between the natural coarse aggregate and
cement paste is observed at 300 days, whereas the ITZ between
these two phases seem disappeared (Fig. 18). The high quantity
of calcium silicate hydrate (CSH) gel formation and the enrichment
of calcium hydroxide (CH) crystals in the ITZ of the control speci-
men produce a dense cement matrix around the natural granite.
This finding indicates a good degree of hydration of the control
concrete.
Figs. 19 and 20, SEM observed a relatively loose and porous ITZ
in RO concrete at age of 28 days and 300 days respectively. SEM
analysis indicated that porous layers and cracks were generated
along the coarse RCA edge with a high concentration of large cal-
cium hydroxide (CH) crystals at this region of the RO concrete.
The porosity near the aggregate surface was measured between
2.6 and up to 3.2 mm (see Fig. 21). The loose and porous ITZ in
RO concrete may be attributed to the following: (i) Higher absorp-
tion capacity of RCA due to the presence of pores and cracks at
adhered mortar on RCA leads to the great absorption of free water
during mixing, thereby causing more water to flow from the
cement matrix to the RCA particle. Consequently, this condition
will contribute less water for hydrating cement in RO concrete,
which allows premature formation in concrete microstructure
and leaving large quantities of calcium hydroxide (CH) crystals in
the pores of ITZ. (ii) Water from the bleeding of RCA that was

Table 7
Chloride concentration of all tested specimens (% of mass of cement).

Specimen No. Chloride concentration (% by mass of cement)

Age of specimens (Days) 90 days 180 days 300 days
Curing Exposure NW SW SW SW
Depths (mm)
CO 0–10 0.100 0.831 0.698 1.064
10–20 0.044 0.133 0.133 0.466
20–30 0.044 0.100 0.067 0.166
30–40 0.022 0.067 0.000 0.133
RO 0–10 0.100 1.264 1.496 1.463
10–20 0.044 0.166 0.765 0.865
20–30 0.022 0.133 0.166 0.399
30–40 0.000 0.100 0.100 0.299
TR 0–10 0.144 0.399 1.164 0.931
10–20 0.067 0.100 0.432 0.399
20–30 0.033 0.033 0.067 0.200
30–40 0.022 0.000 0.067 0.166
304 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306

Cement paste
Cement paste

Dense ITZ

Aggregate

Aggregate

Fig. 18. SEM micrograph of ITZ between natural coarse aggregate and cement paste
of control specimen at 300 days.
Fig. 21. SEM micrograph of ITZ between untreated RCA and cement paste at
300 days (6000 magnification).

not used in the hydration of the cement was evaporated, thereby

forming voids. Analysis confirms that these factors responsible
for the weaker mechanical strength performance of RO concrete
Cement paste
compared with the control. Moreover, the loose and porous ITZ
causes the RO concrete to be susceptible to gas, fluids, or aggres-
Porous ITZ sive ion penetration, thus reducing its long-term durability.
Fig. 22 clearly shows that cracks and voids are also presence at
the old ITZ and old cement paste respectively.
On the other hand, it is found that the ITZ structure formation of
TR is better than that of RO concrete. Fig. 23 shows that despite
loose conjunctions between treated RCA and the hydrated prod-
ucts of cement paste in the ITZ of TR, the pores are smaller in TR
Aggregate than in RO, with sizes that range from 280 nm to 340 nm (see
Fig. 24). The inclusion of surface-treated RCA in the ITZ of concrete
caused the concrete to become denser and more uniform com-
pared with concrete with untreated RCA because of the following
reasons: (i) The wollastonite particles coated with RCA surface pro-
vided an additional layer that absorbs free water during mixing,
Fig. 19. SEM micrograph of ITZ between untreated RCA-paste at 28 days. thereby reducing internal bleeding of water inside the RCA particle.
(ii) Wollastonite particles reacted with cement during the hydra-

Cement paste Old cement paste

Old cement
paste

Porous ITZ
Aggregate Old ITZ

Aggregate

Fig. 20. SEM micrograph of ITZ between untreated RCA and cement paste at
300 days (1000 magnification). Fig. 22. SEM micrograph of old ITZ.
 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306 305

Table 8
Element at EDX spot.

Element Weight% Atomic% Formula

Cement paste C 5.62 9.54 CO2

Al 1.15 0.87 Al2O3
Si 21.35 15.48 SiO2
K 1.52 0.79 K2O
Aggregate Ca 21.25 10.80 CaO

tion process, which consumed calcium hydroxide to increase the

hydration product at the ITZ region. In Fig. 25, the Energy Disper-
sion X-ray (EDX) analysis shows that the hydration products in
that ITZ region have the Ca/Si ratio of 0.99 (see in Table 8). (iii)
Dense ITZ In addition, the formation of new hydrate products can fill and
improve the pore structure of RCA. Thus, the surface-treated RCA
is able to strengthen and improve the ITZ between the aggregate
and the cement paste significantly. Moreover, the presence of
new hydration product formations in the ITZ of TR can prevent
the easy penetration of gas, fluid, or ions into the concretes. This
Fig. 23. SEM micrograph of ITZ between treated RCA and cement paste at 300 days finding supports the statement of the mechanical strength and
(6000 magnification). durability performance of TR concrete is significantly better than
that of RO concrete.

4. Conclusions

From the comprehensive laboratory investigations, some signif-

icant conclusions can be drawn as follows:-
Cement paste
1. The acid treatment followed by wollastonite impregnation on
the RCA able to recover the properties of the used aggregate
and the performance in concrete is comparable to those virgin
aggregate. The RAC containing treated RCA exhibits significant
improvement in compressive strength compared to those mix
with untreated RAC, especially in the marine environment
Aggregate
(SW) exposure. However, SW exposure benefits all specimens
in term of flexural strength. In the ambient (OA) exposure con-
dition, the compressive strength of all specimens is generally
higher than those under prolonged water curing (NW).
2. No significant difference between TR and CO series specimens
in term of water absorption was detected in all exposure condi-
tions. Meanwhile, the water absorption of RO series specimens
Fig. 24. SEM micrograph of ITZ between treated RCA and cement paste at 300 days
was 10% to 35% higher than those CO series for all exposure
(25,000) magnification.
conditions.
3. The differences in intrinsic permeability between the TR and RO
series specimens become gradually significant in the later age.
For the specimens in NW and SW conditions, their intrinsic per-
meability was generally lower than those in OA condition.
4. The porosity in most RAC specimens exposed to SW curing is
lower than other similar mixes exposed to different curing con-
ditions. In addition, the total porosity of the RO series speci-
mens was recorded as the highest among all others in all
kinds of exposure conditions, whereas the porosity of the TR
and CO series was comparable especially in a prolonged curing
period.
5. The result proves that the concentration of chloride ions in all
EDX spot RAC specimens with treated RCA is below 0.4% of the mass of
cement as limited the BS 8110. After 300 days of immersion
in seawater (NW), chloride penetration of the TR series speci-
mens was lower than those of CO series. The chloride content
of the TR series specimens at the depth of 20 mm was managed
to keep below 0.4% but not for CO series. This signifying that the
surface treatment on the RCA was able to enhance the chloride
Fig. 25. EDX spot on new paste matrix side of TR concrete. resistivity of the concrete.
306 S. Ismail et al. / Construction and Building Materials 155 (2017) 296–306
6. The SEM analysis indicated that a relatively loose and porous
concrete were generated at the ITZ between cement paste and
RCA particle in RO specimen, whereas denser ITZ was observed
in control specimen. Meanwhile, the SEM results show that the
surface-treated RCA is able to significantly strengthen and
improve the ITZ between the aggregate and the cement paste.
This result was further proven by the EDX analysis, where
hydration products are detected in the ITZ region.
Acknowledgement
The authors are grateful to Universiti Teknologi MARA, Perak
Branch, Perak, Malaysia and Universiti Sains Malaysia, Penang,
Malaysia for its financial support as well as to all parties that have
contributed in this project.
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