Construction and Building Materials 226 (2019) 72–82

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Construction and Building Materials

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Use of sugarcane bagasse ash sand (SBAS) as corrosion retardant for

reinforced Portland slag cement concrete
Fernando C.R. Almeida a,b,c, Almir Sales a,⇑, Juliana P. Moretti a,d, Paulo C.D. Mendes e
a
Department of Civil Engineering, Federal University of São Carlos, Via Washington Luís, km 235, São Carlos, SP 13565-905, Brazil
b
Institute for Technological Research. Av. Prof. Almeida Prado, 532, Cidade Universitária, São Paulo, SP 05508-901, Brazil
c
Department of Materials Engineering and Construction, Federal University of Minas Gerais, Av. Presidente Antônio Carlos, 6627, Belo Horizonte, MG 31270-901, Brazil
d
Sea Institute, Federal University of São Paulo, Rua Dr. Carvalho de Mendonça, 144, Santos, SP 11070-100, Brazil
e
São Carlos Institute of Chemistry, University of São Paulo, Av. Trabalhador São-carlense, 400, São Carlos, SP 13560-970, Brazil

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

SBAS increases the compressive

strength and chloride penetration
resistance of concrete.

Hydration of slag cements can be
activated by SBAS.

SBAS delays the depassivation of
reinforcing steel (corrosion
retardant).

Incorporation of SBAS up to 30% leads
to a corrosion propagation similar to
that observed for the reference
concrete.

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

Article history: Despite their growing popularity in the construction industry, cement-based materials containing blast-
Received 12 January 2019 furnace slag may be subject to various deteriorative processes including corrosion susceptibility owing to
Received in revised form 4 July 2019 the reduced alkalinity of the cementitious matrix. Sugarcane bagasse ash sand (SBAS), the main agro-
Accepted 19 July 2019
industrial waste in sugar and ethanol production, has the potential to enhance concrete durability.
Available online 29 July 2019
This study aims to evaluate the effect of SBAS as a fine aggregate on the corrosion of reinforced slag
cement concrete. Mixes with different proportions were analysed in terms of mechanical characteristics,
Keywords:
chloride penetration, electrolytic conductivity of pore solution, corrosion potential (by open circuit
Supplementary cementitious materials
Sugarcane bagasse ash sand (SBAS)
potential), and corrosion rate (by polarisation curves and Tafel plot technique), as well as the analysis
Corrosion initiation of the corroded steel bars (by scanning electron microscopy technique). This paper argues the efficiency
Corrosion propagation of SBAS in retarding corrosion up to an optimal content of approximately 30%. SBAS can refine micropores
and act as an alkaline activator of slag cements, leading to increased compressive strength, reduced chlo-
ride penetration depth, and delayed corrosion initiation. Above 30%, the corrosion rate increases, which
could be owing to the modified microstructure and higher electrolytic conductivity of SBAS-concrete pore
solutions, that control the susceptibility of chloride attack on the steel bars.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction

The durability of reinforced concrete used in major infrastruc-

⇑ Corresponding author. ture such as bridges, tunnels, ports, and offshore constructions can
E-mail address: almir@ufscar.br (A. Sales). be severely compromised by corrosion processes. Consequently,

https://doi.org/10.1016/j.conbuildmat.2019.07.217
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82
such damage reduces the service life of the overall structure and sig-
nificantly increases maintenance and repair costs. In the United
States, it is estimated that more than $500 billion (US) is necessary
for rehabilitation of bridges and highway systems, in which the
majority of degradation problems are related to corrosion of rein-
forced concrete [1,2].
This problem refers not only to the corrosion of reinforcing steel
but also to the conditions of protection that the concrete itself cre-
ates around a steel rebar [3,4]. According to Tuutti’s model [5], the
corrosion process in concrete structures comprises two main
stages: initiation and propagation. The first is determined by
changes in the concrete cover as a result of chemical and physical
actions. This cover is responsible for protecting the reinforcement
against neutralising or activating substances with concentrations
favourable for corrosion. Such corrosion begins when deleterious
agents such as CO2 and chlorides penetrate the concrete, usually
through diffusion processes, until the passive environment closest
to the steel is counteracted [6]. When this occurs, the corrosion
mechanisms of the reinforcing steel are initiated, and the propaga-
tion stage begins. In turn, the rate of attack is determined both by
the rate of anode-cathode reactions and the physical contact
between reaction areas [7,8]. As a result, corrosion-induced dam-
ages (e.g. concrete stain, cracking, spalling, delamination, and
cross-section reduction of the reinforcement) may cause aesthetic
deficiency or a decrease in the structural load-bearing capacity
which can lead to the collapse of the structure [1,9].
The durability of reinforced concrete can be optimized through
adequate selection of sustainable materials [10]. It is widely
accepted that supplementary cementitious materials, such as
blast-furnace slag, reduce energetic costs and CO2 emissions from
cement production, improve concrete performance and reduce
wastes from other industries [11,12]. Because of the latent hydrau-
lic property activated by alkalis/lime, slags can effectively replace
up to 95% of ordinary Portland cement [13,14]. However, slags gen-
erally contain fewer alkali compounds and lower hydroxide con-
centrations than pure clinker, leading to reduced pH in
cementitious systems [15,16]. Thus, Portland slag cements can
have a strong effect on the alkalinity of concrete, reducing the pro-
tecting ability against corrosion initiation [17].
In this context, incorporation of alternative materials as fine
aggregates can lead to enhanced durability by means of pore
refinement and increased resistance to the penetration of deleteri-
ous agents [18]. Sugarcane bagasse ash sand (SBAS), a by-product
of sugar and ethanol production, is a potential substitute for natu-
ral sand in cementitious materials [19,20]. Brazil is the world’s lar-
gest sugarcane producer and exporter with an estimated SBAS
generation of 4 million ton/year [21,22]. Previous studies have
shown the potential benefits of SBAS in reducing macropores larger
than 0.1 lm and significantly increasing resistance to chloride pen-
etration in cementitious materials [20,23]. Moreover, the carbona-
tion depths of mortars with up to 30% of SBAS (with respect to the
total sand content) were statistically equivalent to reference sam-
ples [20]. However, the influence of SBAS on concrete durability in
terms of corrosion development, particularly in combination with
supplementary cementitious materials is still unclear and defi-
cient. Therefore, this study aims to evaluate the effect of SBAS as
a fine aggregate in the corrosion process of reinforced Portland slag
cement concrete. Mixes with different SBAS contents were evalu-
Table 1
Chemical composition of SBAS samples in mass, %
Component SiO2 Fe2O3 K2O Al2O3
SBAS before homogenisation 80.2 5.6 4.0 2.6
SBAS after homogenisation 80.8 5.8 3.9 2.5
73
ated in terms of mechanical characteristics and electrochemical
analysis such as corrosion potential and corrosion rate under an
accelerated chloride attack.
2. Materials and methods
In this study, SBAS was employed as a fine aggregate for partial
replacement of natural quartz sand to produce slag cement con-
crete. Three SBAS levels of substitution, in mass, were considered:
0% (reference), 30%, and 50%.
SBAS samples were collected from sugarcane plants in the state
of São Paulo, Brazil, and were submitted to a homogenisation treat-
ment by sieving with a #4.8 mm sieve and grinding for 3 min in a
mechanical mill [19,20]. The chemical compositions of SBAS sam-
ples before and after homogenisation treatment are listed in
Table 1.
Although the equivalent alkali value (Na2O + 0.658 * K2O) for
SBAS (2.8%) is relatively high [24], this content is not harmful for
deleterious expansions triggered by aggregate alkali reactions
[25]. Cementitious matrices with 30% and 50% of SBAS had expan-
sions in the same order of the reference samples, with values far
below the limits required by the Brazilian standard [25,26].
Even after the homogenisation treatment, SBAS had a predom-
inantly crystalline structure of SiO2 a-quartz, as shown by the X-
ray diffraction (XRD) (Fig. 1), previously analysed in [19,20]. The
XRD pattern presents the characteristic peaks of the crystalline
phase and the absence of amorphous halo, justifying the technical
motivation to replace quartz sand by SBAS.
The scanning electron microscopy (SEM) micrographs (Fig. 2)
illustrate the size difference between both aggregates studied.
Table 2 lists the physical characterisation of fine and coarse aggre-
gates used for concrete production.
All samples were prepared using Portland composite cement
with 34%, in weight, of blast-furnace slag (CPII-E32 [28] similar
to CEM II/B-S [13]). Physical and chemical characterisation of Port-
land slag cement is listed in Table 3.
CA-60 steel bars (5 mm diameter and 100 mm length) were
used as working electrodes for electrochemical analysis. For clean-
ing purposes, the steel bars were immersed for 10 min in a 1:1 HCl
aqueous solution with 3.5 g/L of hexamethylenetetramine to con-
trol the acid attack. Then, the bars were brushed, rinsed with deio-
nised water and immersed in acetone for 2 min. Immediately after
drying under a heat gun, the bars were coated with galvanic tape to
delimit the electrode-exposed area (40 mm length cylinder side)
for chloride corrosion (Fig. 3).
The compositions of concrete mixtures are listed in Table 4,
from which three series of concrete with different SBAS contents
were produced [19]. The water/cement ratio (w/c) was slightly
adjusted for each composition to maintain the same consistency
[29], because incorporation of SBAS requires more water in the
mixture [18,30]. This procedure avoided the use of superplasti-
cizer, which could interfere the electrochemical analysis consid-
ered in this study, since techniques to evaluate corrosion may be
very sensitive to different salts present in superplasticizer’s com-
positions [31].
Prismatic samples (50  70  100 mm3) were prepared for elec-
trochemical analysis, considering two treated steel bars (Fig. 3)
embedded in each specimen (Fig. 4). Also, cylindrical samples were
CaO MgO P2 O5 TiO2 Na2O MnO SO3 Loss on ignition
1.8 1.6 1.4 1.4 0.2 0.2 0.1 0.8
1.6 1.5 1.4 1.3 0.2 0.1 0.1 0.7
74 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82

Fig. 1. XRD of SBAS used in this study (blue) after homogenisation treatment (red, Q = quartz) [29]. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of this article.)

Fig. 2. SEM micrographs of fine aggregates: (a) quartz sand; (b) SBAS.

Table 2 Table 3
Characterisation of aggregates used for concrete production. Physical and chemical characterisation of Portland slag cement – CPII-E32 (Source:
manufacturer).
Property SBAS Quartz Basalt
sand gravel Property CPII-E32 Component CPII-E32
(in mass, %)
Specific gravity 2.57 2.45 2.63
Water absorption (%) 0.9 0.5 0.3 Specific gravity 3.02 SiO2 24.1
Maximum dimension (mm) 1.18 6.3 19 Blast-furnace slag content (%) 34.0 Al2O3 7.4
Fineness modulus 1.15 2.32 1.49 Initial setting time (min) 197 Fe2O3 3.1
Quantity of powdery material finer than 75 mm 16.2 0.35 – Final setting time (min) 279 CaO 52.1
(No. 200 sieve) after washing (%) Fineness: MgO 3.4
pH (measured in aqueous solution 1:1, using a 10.4 6.2 – % retained #200 3.60 SO3 2.2
pH-meter, according to [27] – Method A) Blaine specific surface (cm2/g) 4,141 Na2O 0.3
Compressive strength (fcj): K2O 1.1
3 days (MPa) 18.5 Carbonic 1.5
anhydride – CO2
prepared for mechanical and chloride penetration tests. All con- 7 days (MPa) 26.8 Insoluble residue 2.5
crete specimens were compacted by using a vibrating table, 28 days (MPa) 39.5 LOI 1000 °C 4.1
demoulded after 24 h, and cured in climate chamber for 28 days
at a temperature of 21 ± 2 °C and relative humidity of 95 ± 5%
[32,33]. Each concrete composition was tested in triplicate for all variance (ANOVA) and Student’s t-test at a significance level of 5%
tests. were considered for all testing results.
The concrete samples were subjected to aging cycles for The compressive strength test was performed at 28 days (after
22 weeks. Each cycle comprised a week which was divided into a curing) and 182 days (after aging cycles), and carried out by a
wetting semi-cycle in 3.5% NaCl solution for 2 days and a drying servo-mechanical press, at a loading rate of 0.45 ± 0.15 MPa/s,
semi-cycle in an oven at 50 ± 5 °C for 5 days [33]. according to [34]. The compressive strength was obtained from
Table 5 lists the adopted experimental programme according to the average of the ratios between the maximum load of rupture
specimen type, exposure conditions, and age of testing. Analysis of and the cylindrical cross-sectional area of the specimen.
 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82 75

Fig. 3. Steel bar preparation: (a) immersion in hydrochloric acid and hexamethylenetetramine solution; (b) brushing in deionised water; (c) immersion in acetone; (d)
coating with galvanic tape.

Table 4
Mixture composition of concrete samples.

Sample SBAS content (%) Mixture proportion (in mass) Slump test (mm)
Cement Sand SBAS Gravel Water
CR 0 1.000 2.010 – 2.860 0.520 90 ± 5
C30 30 1.000 1.407 0.603 2.860 0.530 87 ± 5
C50 50 1.000 1.005 1.005 2.860 0.540 85 ± 5

Fig. 4. Prismatic moulds of reinforced concrete for electrochemical analysis: (a) positioning of steel bars; (b) concrete-filled moulds with embedded steel bars; (c) open circuit
potential measurement.

Table 5
Experimental programme for concrete samples.

Testing Standard Specimen type Exposure condition Age of testing

Compressive strength [34] Cylindrical Curing only At 28 days
Cylindrical Curing followed by aging cycles At 182 days
Tensile strength [35] Cylindrical Curing only At 28 days
Elastic modulus – Method A [36] Cylindrical Curing only At 28 days
Chloride penetration by colorimetric method with [37] Cylindrical Curing followed by aging cycles At 182 days
AgNO3 and fluorescein
Electrolytic conductivity of pore solution [38] Aqueous solution extracted from powder of Curing followed by drying of At 28 days
concrete specimens concrete specimens
Corrosion potential by open circuit potential [39] Prismatic Curing followed by aging cycles During 22 weeks
after curing
Corrosion rate by polarisation curves [40] Prismatic Curing followed by aging cycles At 182 days
Pitting depth by SEM analysis [41] Extracted steel bars After aging cycles embedded in –
concrete

For the tensile strength test, cylindrical specimens were sub-
jected to diametrical compression according to [35] at 28 days
(after curing). The test was performed using a servo-mechanical
press at loading rate of 0.05 ± 0.02 MPa/s until the rupture. The
tensile strength was determined by Eq. (1).
2P
ft ¼ ; ð1Þ
pDh
where P is the maximum load of rupture (N), D is the diameter of
the cylindrical specimen (mm), and h is the height of the cylindrical
specimen (mm).
The elastic modulus by compressive stress was determined
according to [36] (Method A) at 28 days (after curing). Extensome-
ters were positioned on cylindrical specimens for the strain mea-
surement. The load was applied by a servo-mechanical press at a
loading rate of 0.25 ± 0.05 MPa/s, until the stress corresponding
76 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82
to 30% of the concrete compressive strength (rb) and kept for 60 s.
After that, the load was reduced to a stress of 0.5 MPa (ra) and kept
for 60 s. This process was repeated twice, and, in the last cycle, the
strain was checked for ra and rb, resulting ea and eb. The elastic
modulus was determined by Eq. (2).
rb  0:5
E¼  103
eb  ea
where rb is the stress corresponding to 30% of the concrete com-
pressive strength (MPa), ea is the strain at ra = 0.5 MPa, and eb is
the strain at rb.
The chloride penetration test was conducted using the col-
orimetry method by sprinkling silver nitrate and fluorescein solu-
tion [37]. At 182 days (after 28 days of curing followed by 22 aging
cycles), concrete samples were dried at 105 ± 5 °C and then broken.
The surface obtained by diametrical rupture of the specimen was
treated with 0.1 M silver nitrate (AgNO3) solution and fluorescein
alcoholic solution (1% fluorescein salt, 29% distilled water, 70%
ethanol). A white precipitate (AgCl) was formed after the sprayed
surface dried. This whitish region, in contrast to the darker area,
indicates the presence of chloride ions. The depth of this whitish
area was measured using a digital pachymeter from the outer edge
of the specimen, which indicates the chloride penetration depth in
the concrete specimen.
Electrolytic conductivity was analysed for the pore solution
extracted from finely macerated concrete samples. The extractions
were prepared with a 1:1 proportion (in mass) between the solid
samples and ultrapure water (2.37 mS/cm), during 24 h with occa-
sional agitation, followed by vacuum filtration. The coarse aggre-
gate was not included, since it is expected to release a negligible
quantity of ions [38]. A lab bench conductivity meter, with cell
constant of 0.75 cm1, was used for the measurement at room
temperature.
The corrosion potential was estimated through the open circuit
potential, which was measured in triplicate based on [33,39]. Three
reinforced concrete (prismatic specimens with two embedded
steel bars each) were continuously monitored by means of the
open circuit potential (Eoc) using a high impedance input voltmeter
(Minipa ET-2076). Measurements started at 28 days after the cur-
ing period and were conducted twice a week for both wetting and
drying conditions at the end of each semi-cycle. It was assumed
that the standardisation of the testing condition was obtained
due to the steel bars preparation (Fig. 3) [33]. At the end of 22
cycles, or 182 days after casting, all working electrodes were in
an active state of corrosion, i.e. the Eoc values were inferior to
254 mV vs. the reference electrode of Ag/AgCl/KClsat [39].
At this stage, the polarisation curves were obtained by using a
potentiostat/galvanostat PGSTAT mod. 20 Autolab, using the Ag/
AgCl/KClsat reference electrode and an auxiliary titanium electrode.
This technique is a perturbation method with linear scanning
around Ecorr ± 350 mV at 0.5 mV/s [4,40]. The corrosion current
density (icorr), in lA/cm2, which is directly proportional to the rate
of corrosion, was calculated by Eq. (3) considering the corrosion
potential (Ecorr) and corrosion current (Icorr) obtained from Evans
diagrams and Tafel plots [42,43]:
Icorr
icorr ¼
S down further reaction. If pH is kept sufficiently high in presence of
where Icorr is the corrosion current intensity (lA), and S is the
exposed surface area of the working electrode (15.83 cm2). After-
wards, the steel bars were extracted from the concrete specimens
and were cleaned following the same procedure, as shown in
Fig. 3. The pitting depths of extracted corroded bars were analysed
through the Scanning Electron Microscopy (SEM) technique (EVO
50, Carl Zeiss AG, Oberkochen, German), according to [41]. The sam-
ples were not pre-coated, and observations were carried out in high
vacuum mode, accelerating voltage (EHT) of 15 kV, and working
distance (WD) of 8 mm. The level of corrosion was characterised
by measuring the deepest point of the pitting penetration of each
working electrode [44].
3. Results and discussion
ð2Þ
3.1. Mechanical properties
The results of compressive strength at 28 and 182 days, before
and after aging cycles, as well as those of tensile strength and elas-
tic modulus at 28 days are listed in Table 6.
At 28 days, the incorporation of SBAS increased the compressive
strength by around 8% and 11% for concretes with 30% and 50% of
quartz sand replacement, respectively. At 182 days, the addition of
SBAS resulted in increments of 4% and 14% (absolute values) for
C30 and C50, respectively, relative to the reference concrete (CR).
The considerable increases in strength between both ages must
be attributed to prolonged cement reaction owing to the blast-
furnace slag in the cement composition in addition to the continu-
ous drying/wetting cycles in the saline solution.
The differences between the compressive strength results at
28 days (no aging cycles) are statically significant. The SBAS incor-
poration indeed increased this property even with a higher w/c
ratio for concretes with SBAS. This increment can be attributed
to the packing effect of SBAS in the mixture. According to previous
studies [20,23], SBAS particles have filled pores in size ranges of
60–80 lm and 100–300 lm, resulting in a denser microstructure
and hence increased compressive strength. The increased strength
can also be related to the interaction of SBAS and Portland compos-
ite cement with blast-furnace slag [45].
The reaction of slag itself with Portland cement and water is a
complex process. It is well known that the main constituents of
ordinary Portland cement (PC) are calcium silicates (Ca3SiO5 and
Ca2SiO4), aluminate (Ca3Al2O6), and ferrite (Ca4(AlxFe1-x)4O10)
which can be abbreviated to C3S, C2S, C3A, and C4AF. A number of
other minerals such as calcium sulphates (present as gypsum,
anhydrite and/or hemihydrate), calcite, calcium oxide, magnesium
oxide, Na- and K-sulphates are also usually present. These compo-
nents react with water to form various hydration products such as
calcium silicate hydrate (C–S–H), portlandite (CH), ettringite, cal-
cium monosulphoaluminate or calcium monocarboaluminate
[14,46].
Slag, due to its high alumina and silica content, produces some-
what more complex hydrates than PC. In hydrated PC-slag systems,
the presence of C–S–H, CH, ettringite, AFm (monosulphate and
monocarbonate), and a hydrotalcite-like phases is observed. How-
ever, hydration of PC-slag cements produces less portlandite (at
long term), less ettringite (at high slag content) and less AFm and
AFt phases (as more Al is bound in C–S–H) than in pure PC hydra-
tion. Usually, the C–S–H formed in PC–slag blends has a lower Ca/Si
ratio and a higher Al/Si ratio than pure PC [10]. Introducing alu-
mina into the C–S–H phase, to form C–A–S–H, markedly increases
its alkali-binding capacity and, hence, reduces alkalinity of the pore
solution [47].
In the presence of water, slag hydrates to a limited degree. A
ð3Þ protecting film deficient in calcium is quickly formed, which slows
activators, slag hydration can be accelerated and intensified. The
most common activator of slag is PC clinker, but also other alkaline
materials [48]. In this context, SBAS can act as an alkaline activator,
considering its relatively high equivalent alkali value (Na2O
+ 0.658 * K2O = 2.8%, from Table 1) and higher pH (Table 2) com-
pared to quartz sand. Thus, secondary C–S–H phases can be formed
as hydration products of SBAS-PC-slag concrete, which are respon-
sible for lower permeability and higher strength.
 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82 77

Table 6
Results of mechanical tests of concrete.

Sample Compressive strength (at 28 days) Compressive strength (at 182 days) Tensile strength (at 28 days) Elastic modulus (at 28 days)
(1) (2) (1) (2) (1) (2)
Average SD CV Average SD CV Average SD CV Average SD (1) CV (2)
(MPa) (MPa) (%) (MPa) (MPa) (%) (MPa) (MPa) (%) (GPa) (GPa) (%)
CR 36.54 1.77 5 51.26 1.53 3 3.75 0.11 3 36.96 0.23 1
C30 39.36 1.53 4 53.51 2.94 5 3.70 0.52 14 39.26 1.73 4
C50 40.65 0.67 2 58.74 1.95 3 4.21 0.58 14 37.76 0.65 2
ANOVA and t- CR/C30 & CR/C50 statistically CR/C30/C50 not statistically CR/C30/C50 not statistically CR/C30/C50 not statistically
test significant significant significant significant
(1)
SD: standard deviation.
(2)
CV: coefficient of variation.

Therefore, when slag is mixed with water, its hydration prod-
ucts form a thin Si-rich layer on the surface of the slag grains,
which stifles further hydration [49,50]. In turn, together with port-
landite (CH) and alkali hydroxides from Portland cement hydra-
tion, SBAS can act as slag’s activator. Owing to its higher
alkalinity compared with quartz sand (Table 2), SBAS raises the
pH in the vicinity of the slag and prevents the formation of the
Si-rich layer. As a result, SBAS can improve the hydration degree
of Portland slag cement and increase the compressive strength of
the concrete.
However, according to ANOVA results, the null hypothesis can-
not be rejected for the results of compressive strength at 182 days
(F-statistic < f-critical). Although C30 and C50 reached greater
absolute values than CR, the specimens subjected to degradation
cycles had statistically equivalent compressive strength regardless
of the SBAS content. NaCl salts were crystallised in the concrete
pores, leading to increased compactness in all samples, as shown
in Fig. 5, which led to an increase in the masses of specimens over
the cycles. This effect was caused by the gradual accumulation of
salts into the concrete microstructure in addition to the hygro-
scopic nature of NaCl, which led to increased water retention.
However, the mass increment ceased, and the mass variation sta-
bilised after approximately 16 weeks. This can indicate a ‘satura-
tion’ of the salt crystallisation effect, in which the microstructure
clogging by NaCl potentially overcame the SBAS packing. Thus,
the compressive strength values were statistically equivalent for
concretes with and without SBAS.
The results of tensile strength and elastic modulus at 28 days
were not affected by the SBAS incorporation with F-statistic < f-
critical (p-value > 0.05). However, the evidence was insufficient
for rejecting the null hypothesis by ANOVA test. Thus, the concrete
with SBAS had similar performance for those properties when
compared with the reference sample.
Therefore, SBAS enhanced the mechanical properties by
increasing compressive strength at 28 days. Tensile strength and
elastic modulus, as well as compressive strength after degradation
cycles were not influenced by the SBAS incorporation.
3.2. Chloride penetration
Fig. 6 shows the results of colorimetric testing of chloride pen-
etration in concrete after 22 aging cycles of drying and wetting in
NaCl solution. This qualitative method indicates the presence of
free chloride ions which indeed represent a risk for susceptibility
of reinforcement corrosion.
Analyses through ANOVA and Student’s t-test indicated that all
averages were statistically different. The incorporation of SBAS had
a significant influence on the chloride penetration depth in con-
crete such that a higher SBAS level in the mixture corresponded
to a lower chloride front depth. This result is attributed to the
physical and chemical effects of SBAS.
The physical effect can be related to the filling of micropores with
SBAS particles, particularly pores with dimensions smaller than
150 mm, and the reduction of capillary interconnectivity by adding
a finer material in the mix [20,51]. Moreover, ionic diffusion can
be considered as the main transport mechanism of chloride ions in
concrete with SBAS. The presence of other ions in the pore solution,
such as Na+, K+, Ca2+, and OH, affects the presence of Cl, accelerat-
ing or slowing its penetration via mechanisms of repulsion or attrac-
tion among the electrical charges [52,53]. Thus, incorporation of
finer particles of SBAS affects the transport mechanisms and thus
acts as a barrier against chloride ion penetration.

Fig. 5. Variation in mass of concrete specimens during aging cycles. Higher (lower) values refer to saturated (dried) conditions.
78 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82
Fig. 6. (a) Results of chloride penetration depth and (b) colorimetric treatment applied to concrete specimens.
The chemical effect, in turn, can be attributed to slag activation
by SBAS. The higher pH of SBAS (compared to quartz sand, Table 2)
contributes to activate hydration of Portland-slag cement, result-
ing in the creation of secondary C–S–H. This leads to refinement
of the pore structure and, hence, reduced permeability in the con-
crete [53,54]. Chlorides bind to aluminate phases or are adsorbed
on C–S–H [6]. Therefore, in comparison with the reference con-
crete, the incorporation of SBAS had a positive effect on the resis-
tance to chloride penetration.
3.3. Electrolytic conductivity of pore solution
To improve the understanding of the solution that can be pre-
sent in the pores of the concrete samples, the electrolytic conduc-
tivities of solutions extracted from finely macerated samples (as an
indirect approximation to the pore solution) were compared. The
results are shown in Fig. 7.
There is positive correlation between the conductivity of the
extracted solution and the content of SBAS in the concrete; the
conductivity increased by 14% and 23% for a SBAS incorporation
of 30% and 50%, respectively, with respect to the reference without
SBAS. The conductivity is a summation of contributions from all
ions [38]; however, the increase can be attributed mostly to the
higher concentration of OH expected in the presence of SBAS,
according to the higher associated pH compared with quartz sand
(Table 2). In fact, OH are among the most conductive ions found in
concrete pore solutions [55,56].
The higher conductivity could be expected to facilitate corro-
sion due to the increased mobility of reactive species, i.e., allowing
the flow of electrons and hence corrosion of the reinforcement
bars. However, it is not possible to ascertain the performance of
these materials solely by this measurement, since many other fac-
tors affect the permeability of species and corrosion, such as the
characteristics of the concrete (water/cement ratio, type and pro-
Fig. 7. Results for the conductivity of the aqueous solution extracted from the
cementitious matrix simulating pore solution.
portions of aggregates, cement consumption, the presence of
chemical admixtures, degree of hydration, microstructure and pore
density, rebar passivity, alkalinity of the pore solution); environ-
mental characteristics (temperature and relative humidity) and
the action of aggressive agents (chloride penetration and carbona-
tion) [4,33]. Thus, all properties should be carefully evaluated in
conjunction before reaching a reliable conclusion regarding the
performance expected with SBAS incorporation.
3.4. Corrosion initiation
The results of open circuit potential (Eoc) measured during the
degradation cycles in the saline solution are shown in Fig. 8.
Because the system was allowed time to stabilise before each mea-
surement, the Eoc could be a satisfactory approximation to the cor-
rosion potential for each condition of, specifically the anodic and
cathodic reactions should have the same rate. After 20 weeks, the
probability of corrosion of all working electrodes was expected to
be greater than 90% for all samples with Eoc values below
254 mV versus Ag/AgCl (saturated KCl) [39].
The outliers observed during the first week can be attributed to
the dramatic change in environment from a humidity chamber
with curing at 95% relative humidity to aging cycles in a saline
solution. However, during the following weeks, all measurements
stabilised, indicating a trend related to the wetting and drying
cycles to which the concrete samples were subjected. The varia-
tions in the Eoc measurements for each semi-cycle were attributed
to the moisture content of the specimens, directly affecting the
ohmic drop in the concrete. Specifically, less negative Eoc values
were obtained after drying semi-cycles in which the electrical
resistivity or the difficulty of ion movement was higher, whereas
the Eoc was more negative when the samples were saturated with
the solution. This is because the minimized ohmic drop under sat-
uration condition led to lower electrical resistivity, resulting in
more negative Eoc values [57].
Overall, during the passivation period, working electrodes pre-
sented Eoc values between 160 mV and 30 mV. At the time of
depassivation (Eoc < 254 mV), a sharp decline in Eoc values was
verified for all samples, indicating the beginning of corrosion prop-
agation in the steel bars [33]. The working electrodes in the refer-
ence concrete were the first bars to begin corrosion propagation, at
week 14, followed by concretes C50 and C30 at weeks 16 and 18,
respectively. The delay in corrosion activation in the steel bars
may be related to the packing effect of SBAS. The substitution pro-
portion of 30% must have contributed as an ideal condition to close
or interrupt the connectivity between pores [20,23]. This created a
physical barrier against the attack of chloride ions [58]. Moreover,
the increment of alkalinity in the concrete by SBAS may have con-
tributed to delay corrosion initiation. Concrete samples CR, C30
 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82 79

Fig. 8. Evolution of the open circuit potential of working electrodes versus Ag/AgCl/KClsat in concrete specimens.

and C50 respectively had pH values of 11.93, 12.32 and 12.33, mea-
sured by this research group from the solubilised extracts [19,25]
obtained according to the Brazilian standard [59]. The susceptibil-
ity to pitting corrosion in an acid solution containing primarily
chlorides increased with the decreased alkalinity provided by the
passivation cover [6,60], i.e. the balance between alkalinity and
acidity, given by the activity of OH and Cl, respectively, is
responsible for maintaining the passivation of the reinforced rebar.
In summary, the beginning of the corrosion process in reinforced
concrete was delayed by substituting 30% of the quartz sand with
SBAS, owing to its physical influence in refining micropores and its
higher alkalinity.

3.5. Corrosion propagation

The linear polarisation curves are shown in Fig. 9, where the

current values (I) are plotted against the overpotential (g),
obtained by sweeping at 0.5 mV/s, from the lower limit around
the Eoc following the relation g = Eoc ± 350 mV. Analogous to the
interpretation of Eoc, the Ecorr indicates the electrochemical
dynamic equilibrium, in which both the anodic and cathodic cur-
rents have the same magnitude and thus the resultant total current
is null. From this point, the anodic and cathodic terms are unbal-
anced by the application of overpotentials, where the polarisation
resistance and current propagation can be interpreted. Although
ohmic drop is one of the main error sources of this technique
[4,57], it was minimised by employing samples which were
already corroded after conditioning cycles (Fig. 8) and were fully
saturated with NaCl solution electrolytes.
Active dissolution of the working electrode was noted for all
samples, as indicated by the upward sloping curve in relation to
the overpotential axis. In particular, sample C50 presented the
highest current values according to its highest slope, both in the
anodic branch (positive values of g) and cathodic branch (negative
values of g) indicating greater dissolution of the metal. Specimens
CR and C30 had profiles similar to each other when compared with
C50, although their current was significantly lower. It is crucial to
keep in mind that the current is proportional to the electrode area.
Although the exposed geometric area was the same for all samples,
the unique corrosion process that occurred on each material
greatly affects this measurement, hence, a higher active area could
be expected for C50 to explain the higher currents. The corrosion
Fig. 9. Polarisation curves of working electrodes in concrete (linear scale).
rates are directly proportional to the corrosion current, i.e. higher
values of electrical current passing through the system indicate
that the corrosion is more severe. Thus, by a qualitative analysis,
it can be inferred that the corrosion propagation was greater for
C50 and was similar for CR and C30.
To determine the corrosion current, the polarisation curves
were plotted in a logarithm scale (Evans diagram, Fig. 10). From
the intersection of the extended cathodic and anodic branches on
the Tafel slope, the corrosion potential (Ecorr) and corrosion cur-
rent, or more accurately, the logarithm of the corrosion current
(log |Icorr|) were found. This result, in turn, can be extrapolated to
corrosion rate analysis by considering the following factors: (i)
generalised corrosion, which is perfectly uniform along the sur-
face; (ii) simple dissolution as the only anodic reaction, written
as Fe0 ? Fe2+ + 2e; and (iii) Faraday’s constant. The results of
the corrosion current density (icorr) of each working electrode are
listed in Table 7.
The results emphasise the similarities between CR and C30
samples, which had the same order of corrosion current density.
Because they were in the range of 0.5–1.0 lA/cm2, both rates could
be classified as moderate levels but not severe [44]. However, C50
clearly had the greatest corrosion propagation compared with the
80 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82

Fig. 10. Evans diagrams and Tafel plots: polarisation curves of working electrodes
in concrete (logarithm scale).

other two samples, with a rate about 10 times greater than the rate
of the reference sample. C50 can be characterised as have a high
level of corrosion because its icorr value was greater than 1.0 lA/
cm2 [44].
It is worthwhile to note that the approximation of the corrosion
rate is affected by how localised the corrosion is. As mentioned
above, this corrosion rate analysis is extrapolated by considering
Fig. 11. SEM micrographs for typical pitting depth measurements. The inserts show
a generalised corrosion, which is perfectly uniform along the steel the pointed cavities of each working electrode (reinforcing steel bars) in detail.
surface. However, the presence of pitting, cracks and other surface

Table 7
Results of corrosion parameters of working electrodes in concrete samples.

Sample Ecorr (mV) log |Icorr| Icorr (mA) icorr (mA/cm2) Pitting depth by SEM (mm) Classification by [44]
CR 600.2 4.9 11.6 0.7 242.4 moderate
C30 663.2 4.9 13.7 0.9 238.0 moderate
C50 686.6 3.9 121.2 7.7 460.4 high
 F.C.R. Almeida et al. / Construction and Building Materials 226 (2019) 72–82
irregularities need to be evaluated carefully to further understand
the results.
In this context, the typical pitting depths of corroded steel bars
were characterised by the SEM micrography technique (Fig. 11).
The steel bars embedded in concrete C50 had the greatest surface
irregularities (pitting depth) in comparison with the other samples
(Table 7), indicating a more localised corrosion. If the remaining
areas of the steel bar are considered passive, a high corrosion cur-
rent divided by a smaller area (more localised) results in a higher
corrosion current density. This technique completes the under-
standing of the corrosion profile, because the analysed working
electrodes did not incur uniform and generalised degradation. As
expected, the corrosion was localised, which is characteristic of
the chloride action and indicated by the cavities on the bar surface.
Pitting corrosion can be more dangerous than uniform deteriora-
tion because it progressively reduces the cross-sectional area of
the rebar to a point at which it can no longer withstand the applied
load, leading to severe structural failure [4].
Increments of corrosion kinetics in concrete with SBAS, particu-
larly at contents above 30%, can be related to its increased elec-
trolytic conductivity (Fig. 7). Moreover, the presence of some
salts in the matrix, such as NaCl from saline solution during the
aging cycles, accelerates the electrochemical reactions on the steel
bars during corrosion progress. This is owing to their capacities for
depolarising and, consequently, increasing the electrical charge
passing through the concrete as an effect of dissolved salts. In this
context, particularly C50 had the greatest mass variation on the
wetting and drying cycles (Fig. 5), indicating a higher water
absorption capacity (including saline solutions) and, hence, a
greater ability of NaCl crystallisation. Thus, incorporation of higher
SBAS levels of more than 30% can contribute to faster propagation
of the corrosive process, especially due to the modified microstruc-
ture of the cementitious matrix and increased ionic mobility in the
mix which leads to greater electrolytic conductivity.
Although SBAS may retard the beginning of the corrosive pro-
cess, as indicated by Eoc measurements, this by-product con-
tributed to accelerating the corrosion propagation as soon as it
began. This negative effect was even more pronounced in concrete
with 50% SBAS. Therefore, incorporation of SBAS at levels up to 30%
can reduce corrosion probability, as a retardant of corrosion initia-
tion, and keep corrosion propagation at the same rate as the refer-
ence sample. Moreover, it has been well identified that not only the
corrosion rate is important but also how localised it is. Due to the
limited number of samples to deduce a ‘‘Tuutti’s prediction” [5]
and adverse conditions in field, the outcomes presented herein
may not occur in practice. However, this study is representative
of general trends that can be expected and is important for basing
the advances of the current knowledge on reinforcement corrosion
of SBAS concrete.
4. Conclusion
On the basis of the results obtained in this experimental study,
the following conclusions were drawn:

The substitution of quartz sand by SBAS increases both the com-
pressive strength and resistance to chloride penetration of con-
crete. This positive outcome can be attributed mainly to a
packing effect and the ability of SBAS to act as an alkaline acti-
vator to Portland-slag cement. The tensile strength and elastic
modulus are not significantly affected by the incorporation of
SBAS.

The incorporation of SBAS leads to decreased probability of cor-
rosion, owing to the delayed depassivation of the reinforcing
steel. This effect is related to increased concrete alkalinity and
decreased pores connectivity promoted by SBAS. Concrete with
81
approximately 30% of SBAS seems to indicate an appropriate
mixture for retarding the initiation of corrosive processes.

Once corrosion began, the propagation rate is higher for con-
crete with SBAS contents greater than 30%, due to the modified
microstructure and increased conductivity of its pore solution.
It appears that a SBAS content of about 30% may result in a
physical and electrochemical balance between closing microp-
ores (or interrupting pores connectivity) and satisfying an ade-
quate conductivity of the pore solution that controls the
susceptibility of chloride attack on the steel bars. This equilib-
rium prevents the propagation of higher corrosion currents
and creates a propagation condition comparable to the beha-
viour for a sample without SBAS. For future studies, evaluating
different SBAS concentrations around 30% is recommended in
order to accurately identify the optimal content that leads to
an enhanced concrete performance.
Therefore, in addition to environmental benefits of reusing an
agro-industrial by-product, the incorporation of SBAS at levels up
to 30% can improve the mechanical properties and enhance the
durability of reinforced concrete. The capacity of SBAS to retard
corrosion initiation in an environment susceptible to chloride
attack adds value to this new eco-friendly construction material.
Declaration of Competing Interest
There is no conflict of interest.
Acknowledgments
The authors acknowledge CAPES 001 and CNPq (Grant numbers
309892/2013-9 and 409685/2017-8) for financial support, Cosan
for SBAS supplies, and Prof Lucia H. Mascaro from Laboratório
Interdisciplinar de Eletroquímica & Cerâmica (LIEC/UFSCar) for
electrochemical measurement support.
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