Construction and Building Materials 404 (2023) 133267

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Construction and Building Materials

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

Durability of concrete incorporating recycled coarse aggregates:

carbonation and service life prediction under chloride-induced corrosion
Tiago Luis Possebon Ortolan a, Pietra Moraes Borges a, Laura Silvestro b,
Sérgio Roberto da Silva a, Edna Possan c, Jairo José de Oliveira Andrade a, *
a
Graduate Program of Materials Engineering and Technology, Pontifical Catholic University of Rio Grande do Sul (PGETEMA/PUCRS), Brazil
b
Federal University of Technology – Paraná (UTFPR), Brazil
c
Graduate Program of Civil Engineering, Federal University of Latin-American Integration (UNILA), Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: The use of recycled aggregates (RA) is growing due to the environmental problems associated with extracting
Construction and demolition waste natural aggregates (NA) and the disposal of construction and demolition waste (CDW). However, the service-life
Recycled aggregate prediction of recycled coarse aggregate concretes remains incipient. Thus, this study aimed to evaluate the effects
Carbonation
of different replacement contents of NA by RA (25, 50, and 75 wt%) on physical (water absorption, porosity, and
Chloride
bulk density), mechanical properties (compressive strength and modulus of elasticity), microstructure (evaluated
Service-life prediction
Surface protection systems by X-ray microtomography), accelerated carbonation, and chloride penetration of concrete. A service life pre­
diction analysis of RA concretes was conducted based on the chloride profile obtained and considering the
application of different concrete surface treatments. The RA contents evaluated increased the carbonation and
chloride diffusion coefficients by 75.7% and 43.0%, respectively, compared to the reference concrete. Never­
theless, reductions of approximately 50% on the critical chloride concentration depth of RA concretes are esti­
mated considering the application of acrylic-based surface treatment. Therefore, applying surface treatments is
promising to increase RA concretes’ durability and service life, contributing to its wide use and dissemination
feasibility.

1. Introduction
Human society has faced considerable challenges in controlling
greenhouse gases, making it an international agenda in governments
and industries. The basis of this commitment was made in the Paris
Agreement in 2015 [1]. Specifically in Europe, the European Green Deal
[2] established 2050 as the critical year for carbon–neutral projects.
According to the World Population Prospects report [3], presented by
the United Nations, the global population will reach 9.7 billion in 2050,
and 68% will live in urban areas. The increase in the urban population
will lead to a proportional increase in demand for transport and logistic
infrastructure, just like homes and leisure areas in the big cities.
The construction industry is a big consumer of aggregates that are
applied in producing concretes and mortars. The aggregate extraction
and beneficiation process can cause much environmental damage. The
transportation expenses incurred in moving natural aggregates (NA)
from extraction points to important centers, coupled with the resulting
CO2 emissions, may pose challenges for the sustained extraction of such
materials. Thus, recycled aggregate (RA) from construction and demo­
lition waste (CDW) is an interesting alternative for the previously pre­
sented problems. In Brazil, [4] the volume of CDW collected was
approximately 48 million tons in 2021, 3.0% higher than the last year
(2020). According to Huang et al. [5], this waste volume is primarily
disposed of in landfills, causing environmental impact by the extensive
land use and transportation from the urban centers. Furthermore, only
6.0% of the CDW generated is recovered [6], evidencing that the country
needs to combine efforts to encourage and enable higher reuse rates and
the wide dissemination of RA.
Much research has been done about RA’s applicability in concretes
and mortars, and the results are essentially promisor, demonstrating the
viability until a determinate replacement level [7–10]. However,
employing these materials can cause adverse effects on some concrete
properties. Many researchers verified the decrease in compressive
strength and elastic modulus. This occurs mainly due to some factors:

* Corresponding author.
E-mail addresses: tiago.ortolan@edu.pucrs.br (T.L.P. Ortolan), pietra.borges@acad.pucrs.br (P.M. Borges), laurasilvestro@utfpr.edu.br (L. Silvestro), sergio.
roberto@acad.pucrs.br (S.R. da Silva), epossan@gmail.com (E. Possan), jairo.andrade@pucrs.br (J.J.O. Andrade).

https://doi.org/10.1016/j.conbuildmat.2023.133267
Received 21 May 2023; Received in revised form 26 August 2023; Accepted 5 September 2023
Available online 12 September 2023
0950-0618/© 2023 Elsevier Ltd. All rights reserved.
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

the inherent variability of RA, considering the locality; type of CDW showed that the service life of concretes investigated increases signifi­
(concrete, ceramic and mixed) that origin the RA; the particle charac­ cantly with protective coatings. However, the application of surface
teristics, like the amount of mortar adhered in old particles of aggregates treatments to mitigate the adverse effects of RA on the durability of
that influence in porosity, permeability, and interfacial transition zone; concrete has not been widely discussed regarding chloride-induced
and the processing activities, like crushing and washing [11]. corrosion. Thus, this study has three main objectives: (i) evaluating
Along with the mechanical properties, evaluating the durability of the effect of different replacement contents of NA by RA on the me­
concretes with RA is important to evaluate their potential use. To chanical properties and microstructure of concretes, (ii) the impact of
investigate the service life prediction is fundamental to ensure adequate RA on the service life of concretes in terms of carbonation of chloride-
performance levels of concretes when inserted in environments with induced corrosion and (iii) simulating different types of surface treat­
CO2 and chloride ions [12]. In several standards and codes of practice, ments to mitigate the negative impact of RA in chloride penetration and,
the service life is related to the corrosion of reinforcement, which is a thus, viability its use in concrete.
phenomenon that occurs in several concrete structures with catastrophic
consequences. This phenomenon presents mainly two stages: the initi­ 2. Experimental procedure
ation (related to the diffusion of chloride ions and CO2 into pore struc­
ture, leading to the depassivation of reinforcement) and the propagation 2.1. Materials
(considering the loss of a section of reinforcement leading to loss of
adherence, displacement and in some cases the collapse of structure) The Portland Cement (PC) utilized for concrete production was the
[13]. Both stages are worrisome and influence the service life. It is Brazilian CPV-ARI [32], like ASTM C 150 III, with a specific surface of
imperative to know the characteristics of the concrete constituent ma­ 3.07 g/cm3, bulk density of 1.04 g/cm3 mean particle size of 14.16 μm
terials that can maximize the initiation period, which is generally and mean compressive strength at 28 days of 54.10 MPa. The concretes
considered the design service life of a structure [14]. Ashraf et al.[15] were produced using sand as fine NA. Two types of coarse aggregate
verified that the chloride diffusion coefficient of RA presents a certain were evaluated: the natural basaltic (NA) and the recycled aggregate
level of fluctuation due to the old mortar attached to the aggregate. (RA) from the processing of a CDW obtained from a demolition site in
Neves and Brito [16] reported progressive reductions in the service life Porto Alegre, Brazil. The CDW was classified, removing contaminants
of concretes with the increase in replacement content of NA by recycled such as paper, wood, plastics, and polymers, and before crushing the
coarse aggregate. Reductions in service life predictions of up to 32% and composition the RA presented 35% ceramics, 42% mortar, 10% natural
19% were observed for carbonation and chloride-induced corrosion, aggregate, and 14% old concrete. The results of the physical charac­
respectively, for a total replacement of NA by RA [16]. terization of the aggregates were obtained based on Brazilian standards,
Many studies have proposed to establish a relationship between the as shown in Table 1.
variables that influence the various transport mechanisms in porous The chemical composition, determined by X-ray fluorescence (XRF)
materials, aiming to obtain formulations for estimating the design life of for PC and RA, is shown in Table 2. The particle size distribution of
a structure [17–19]. In this way, Possan, Andrade and Dal Molin [20] coarse (a) and fine (b) aggregates is presented in Fig. 1.
proposed a conceptual framework to predict the service life of concrete The mineralogical composition of RA was determined by X-ray
structures, considering several environmental characteristics and prop­ diffraction (XRD) using a brand diffractometer Panalytical, model
erties. The classical square root model proposed by Tuutti [23] for Empyrean, with radiation Cukα, λ = 1.5418, between 10◦ and 80◦ of 2θ,
carbonation is widely used. At the same time, for chloride penetration, are presented in Fig. 2. The data were interpreted with pattern data in
the mathematical modeling based on the solution of Fick’s second law Crystallography Open Database. As can be seen, RA is composed pre­
and derivations is employed [21]. Nevertheless, most of the prediction dominantly of quartz and calcite.
models rely on research conducted on NA concrete, and there is a
scarcity of studies that examine the corrosion in RA concretes [22]. 2.2. Compositions of concrete mixes
Usually, regarding chloride-induction corrosion, accelerated evalua­
tions based on rapid chloride migration tests are employed [23]. How­ The ABCP/ACI method [36] was used to mix proportioning the
ever, in these cases, the dominant transport mechanism is migration concretes. It was defined as compressive strength of 30 MPa at 28 days,
caused by an electric field, unlike what occurs under normal conditions, with consistency equal to 110 ± 10 mm with a 0.5 water-to-cement (w/
i.e., ion diffusion, promoted by a concentration gradient [24]. Addi­ c) ratio. It was considered a weight compensation for the NA and RA
tionally, although some studies have comparatively evaluated the per­ based on the differences between physical properties. The compensation
formance of RA compared to NA concerning chloride-induced corrosion, is presented in Equation (1), as proposed by many authors [37–39].
the impact of these aggregates on the service life of concrete has not
γRA
been fully explored [25–28]. MRA = MNA × (1)
γ NA
Some protective procedures that can be applied to extend the service
life of concretes when inserted in marine environments are widely Where: MRA = Recycled aggregate weight (kg), MNA = Natural
known. The use of corrosion inhibitors in hardened concrete surfaces, an aggregate weight (kg), γ RA = Recycled aggregate specific surface (kg/
electrochemical method for chloride extraction, protective coatings for dm3), γNA = Natural aggregate specific surface (kg/dm3).
steel bars with epoxy, and cathodic protection have been studied in To minimize the impact of water absorption, the recycled aggregate
recent years [29]. Surface protection films – mainly acrylic and silane/
siloxane emulsions – are technically and economically viable alterna­ Table 1
tives to maximize a structure’s service life. This material type forms a Characterization of the aggregates.
thin layer in concrete surfaces with low permeability and diffusivity.
Aggregate Specific Bulk density Fineness Maximum size
Some investigations were made to evaluate the performance of these type gravity (g/cm3) modulus (mm)
materials. Medeiros and Helene [30] verified that a polyurethane NBR NM NBR NM NBR NM NBR NM
coating reduces in 86% the diffusion coefficient of concretes by 53 [33] 45 [34] 248 [35] 248 [35]
extending the service life 7 to 8 times. In recent years, several in­ Sand 2.62 1.61 2.76 4.75
vestigations have been underway to improve surface protection mate­ NA 2.81 1.55 7.01 19
rials’ performance, including developing new ones. Li et al. [31] RA 2.46 0.98 6.84 19
developed a nanopolymer-modified cementitious coating, with nano- Where NBR = Brazilian technical standard; NA = Natural coarse aggregate; RA
TiO2 and nano-SiO2 dispersed in an acrylic emulsion. The authors = Recycled aggregate.

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T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Table 2
Chemical composition and physical properties of PC and RA.
Material SiO2 (%) TiO2 (%) Al2O3 (%) Fe2O3 (%) MgO (%) CaO (%) K2O (%) SO3 (%) LOI*

PC 17.78 0.18 3.92 2.91 4.08 61.96 0.78 3.28 5.42

RA 58.11 0.64 10.01 3.57 2.10 11.57 1.67 0.38 10.78

*Loss on Ignition, PC = Portland Cement, RA = Recycled aggregate.

Fig. 1. Particle size distribution: RA and NA (a); fine aggregate (b).

Fig. 2. XRD for RA.

was immersed in water for 24 h and superficially dried before concrete
production. The RA had 5.8% water absorption. Table 3 presents the mix
proportioning for the concretes and the nomenclature defined for each
mix design.
2.3. Test methods
2.3.1. Mechanical and physical properties
The specimens were demolded after a 24-hour curing process
immersed in water. The characterization process was performed with
tests according to Brazilian and international standards, as presented in
Table 4.
2.3.2. X-ray microtomography
Cylindrical samples of approximately 2.5 cm in diameter and 5 cm
high were collected from REF, and 75% RA concretes at the age of 210
days. The analysis was performed in a Bruker SkyScan 1173 model,
equipment with an operational energy of 50 kV and an electric current of

3
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Table 3
Concrete mix compositions.
Mix design Proportioning (C:S:NA:RA)* Cement (kg/m3) Sand (kg/m3) Coarse aggsregate (kg/m3) Consistency (mm)

NA RA

REF 1:1.97:2.9:0 390 768.3 1,131.0 0 165

25% RA 1:1.97:2.18:0.61 390 768.3 850.2 237.9 135
50% RA 1:1.97:1.45:1.21 390 768.3 565.0 471.9 155
75% RA 1:1.97:0.73:1.82 390 768.3 284.7 709.8 155

Table 4
Test methods used.
Properties evaluated Specimens Brazilian Age
Standard (days)
Number Dimensions
(cm)

Compressive Strength 8 Cylindrical NBR 5739 7, 28, 63,

10 × 20 [40] and 91
Elastic Modulus 9 Cylindrical NBR 8522 28, 63,
10 × 20 [41] and 91
Carbonation depth 1 Prismatic Procedure 63, 91,
10 × 10 × 30 adopted by da 120, 150,
Silva et al. 180, and
[42] 210
Chloride penetration 2 Prismatic Lab Procedure 28, 56,
10 × 10 × 30 84, 112,
and 140
Absoption by 2 Cylindrical NBR 9778 28
immersion, porosity 10 × 20 [43]
and bulk density
X-ray 1 Cylindrical Lab procedure 210
microtomography 2.5 × 5

0.3 mA. The test consists of slicing the sample into hundreds of 2D im­
ages, then using DataViewer Software to define an area of interest of 1
cm × 1 cm × 1 cm to observe in a 3D model. Zhang [44] used the same
technique to analyze the microstructural progress involved in the cure
period of cementitious materials. The same methodology was also
applied by Nunes [45] to observe the RA influence on the concrete
microstructure.

2.3.3. Accelerated carbonation

After 28 days of submerged cure, the concretes were inserted in a
Fig. 3. Test procedure for determining the chloride content: (a) sample
carbonation chamber with 3% CO2 concentration and humidity of 60 ± collection, (b) dilution of samples in deionized water using a magnetic stirrer,
10% to measure the carbonation depth. With 63 days of exposure, the and (c) analysis of chloride content by direct potentiometry.
concretes were sliced with 5 cm, where a solution of 1% phenolphtha­
lein was applied. Immediately, the concrete specimens were photo­
analyzed by direct potentiometry, as shown in Fig. 3(c).
graphed, and the carbonation depth of the faces was determined using
Following the procedure proposed by Haque and Kayyali [47] the
the ImageJ software. Five measurements were taken for each lateral
free chloride analysis was determined by a direct potentiometry test.
face, totaling twenty values for each specimen.
The free-chloride test was chosen because it is responsible for the
corrosion process. Otherwise, direct potentiometry is used to ease
2.3.4. Chloride ion penetration
obtaining results, access to necessary material, and the standardization
Two prismatic concrete samples (10 × 10 × 30 cm) were kept in a
available. The sample collection methodology is presented in ASTM C
submerged cure for 28 days and then were withdrawn and kept in a
1152 [48] and RILEM TC 178-TMC [49]. The equipment was a model
protected and covered environment for seven days to dry. In this period,
CL–3000 by NDT James Instruments. The test requires a calibration
four faces (two 10 × 10 and 10 × 30 cm) were impermeabilized to
process with five aqueous solutions of known chloride concentrations,
prevent the chlorides from penetrating in both directions, and the other
making it possible to create pattern curves. The chloride concentration
two faces were kept unprotected, guaranteeing a unidirectional advance
obtained by concrete weight was initially transformed to cement weight
of chlorides. After seven days, the samples were immersed in NaCl so­
using Equation (2) [50]. Previous studies reported in the literature
lution with a concentration equal to 3.5% [46]. At the ages in Table 4,
adopted the same equation for this conversion [51]. Furthermore, the
the prismatic samples were removed from the solution, dried in a lab­
chloride concentration by cement weight is comparable to applicable
oratory environment, and collected powered samples to determine the
standards [52,53].
chloride content at each 1 cm. Was used an impact drill BOSCH GBH 2-
24D to collect seven different samples of the same age, one for a depth of (Clcement xCc )
ClConcrete = (2)
analysis (1, 2, 3, 4, and 5 cm) as shown in Fig. 3(a). After each sample γc
collection, the holes were filled with impermeabilizing mortar. Subse­
Where: ClConcrete = Chloride concentration by concrete weight (%);
quently, the samples were diluted in deionized water (Fig. 3(b)) and
Clcement = Chloride concentration by cement weight (%); γc = Concrete

4
T.L.P. Ortolan et al.
Specific gravity (kg/m3); Cc = Cement content (kg/m3).
The chloride concentration by cement weight was used to calculate
the concrete’s diffusion coefficient (D) and surface concentration (Cs).
This process was done by adjusting the values obtained experimentally
by applying the solution of Fick’s second law (Equation (3). This
adjustment was made through a non-linear regression combined with
the least square method using the Solver tool, as used in previous studies
[51,54]. The input data were the sample depth (cm), exposure time
(years), and the chloride concentration obtained. A maximum difference
of 5% between the calculated experimental data was established for the
adjustment, ensuring a good fit for determining Cs and D of concretes
with NA and RA.
[ ( )]
x
C(x, t) = Cs × 1 − erf √̅̅̅̅̅̅̅̅̅̅ (3)
4.t.D
Where: C(x,t) = chloride concentration at deep x at time t; Cs =
Superficial concentration (%); erf = Gauss error function; x = Depth
(cm); t = Time (years); D = Diffusion coefficient (cm2/year).
2.3.5. Service-life prediction
Fick’s error function is suitable for performing adjustments of chlo­
ride profiles obtained through experimental data (either in the labora­
tory or in the field). However, it does not consider the variation of Cs and
D over time. Therefore, changes must be made in the original expression
over time, aiming to incorporate this premise to estimate the project
service life of concretes. To consider the decrease of D over time due to
the continuous microstructural densification resulting from hydration
processes was used the expression proposed by Mangat and Molloy [55]
(Equation (4).
(t )m
(4)
ref
D(t) = Dref ×
t
Where: D(t) = Diffusion coefficient at time t (cm2/year); Dref =
Diffusion coefficient at the reference date (cm2/year); tref = Time
associated with Dref (years); t = Time (years); m = empirical coefficient
in the function of time.
Concerning the behavior of Cs, Costa and Appleton [56] proposed
Equation (5), assuming a tendency for a rapid increase in Cs at early ages
and stabilization of this parameter throughout the structure’s service
life.
Cs (t) = Csref × tn
Where: Cs(t) = Surface concentration at time t (% cement weight);
Csref = Surface concentration at the reference date (% cement weight); t
= Time (years); n = Empirical coefficient as a function of time.
In addition, to evaluate the effectiveness of surface protection sys­
tems in the service life of concretes were used the results obtained by
Medeiros e Helene [50] (Table 5). The authors cast concretes with w/c
equal to 0.55, immersed the samples in a solution with 3% NaCl for 319
days, and collected samples to determine the chloride content. The au­
thors used the 2nd Fick’s Law solution to adjust the chloride profiles,
showing a decrease of D.
Thus, the probable values of D associated with the surface protection
systems were calculated to estimate the service life of concretes with
different RA contents.
Table 5
D values for different surface protection systems [50].
System Product D (cm2/year) Decrease of D
None – 0.700 – The reference sample presented a porosity equal to 1.51%, calculated
A Silane/siloxane dispersed in a solvent 0.215 69%
B Acrylic dispersed in solvent 0.182 75%
Construction and Building Materials 404 (2023) 133267
3. Results and discussions
3.1. Physical properties
Table 6 presents the analysis of variance (ANOVA) for physical
properties considering the variation provided by the changes in the
replacement content of NA for RA.
The results showed that varying the replacement content of NA by
RA significantly changed all the physical properties evaluated. The F-
test also observed that the property with the more significant changes
according to the RA replacement level was the specific gravity. This
happens because the RA is lighter than the natural one. The behavior of
these properties is shown in Fig. 4.
It can be observed that the porosity and water absorption by im­
mersion follow the tendency to increase in function of RA replacement
level. The sample with 75% RA is 28% more porous than the reference
one, and the absorption by immersion was 43% higher. Overall, the RA
exhibited a lower specific gravity (Table 1) and, consequently, higher
water absorption than NA. These results are consistent with existing
literature [57]. The residual adhered mortar of RA and the roughened
surface and angular shape of this type of aggregate enhance interparticle
friction, leading to a higher water demand [58].
3.2. Mechanical properties
The mechanical properties were evaluated through compressive
strength and elastic modulus. It is verified by ANOVA (Table 7) that RA
replacement level and age × RA replacement have significance in the
compressive strength and the elastic modulus for both ages. Through the
F-test, the RA replacement level has more influence on the results than
the concrete age. Fig. 5 shows all the results obtained.
The results obtained for compressive strength (Fig. 5a) are like others
found in the literature [9,59–61], where the concretes present a
decrease in the compressive strength with the increase in the RA
replacement content. The 50% RA concrete had lower compressive
strength, 14.9% inferior to the reference one. The 25% RA concrete
presented value is lower than REF (7.9% at 28 days and 13.8% at 210
days). There is no pattern for a decrease, but this can happen due to the
RA heterogeneity, higher porosity, and water absorption.
The RA concrete showed stability of compressive strength growth by
(5) 63 days. However, reference concrete keeps gaining strength after 91
days. Cantero et al. [60] also obtained similar results where concretes
with 50% RA presented compressive strength 25% lower than the
reference one. Bravo et al. [62] conclude that concretes with 100% RA
performed 21.5% to 31.6% lower. However, concretes with 10% RA
didn’t present a significant decrease in the mechanical properties.
To the elastic modulus (Fig. 5b), the 75% RA concrete is 34.6% lower
than reference concrete. The higher porosity of recycled aggregates
corroborates the decrease in the elastic modulus [63], which also
affected the density of concretes with RA (Fig. 4). The same tendencies
are presented by some researchers [10,64]. Adessina[59] evaluated the
RA influence on microstructural characteristics, concluding that old
mortar and cement paste fragilized the new transition zone, lowering
compressive strength and elastic modulus.
3.3. X-ray microtomography
The images obtained in the X-ray microtomography are present in
Figs. 6 and 7. The images represent a) the area of interest reconstructed,
presented in light grey the coarse aggregate and in grey the mortar; in
black, it is possible to observe the sectioned pores, and b) the recon­
structed image of only the pores present in the sample, present in the
mortar and RA.
with the reconstructed image. The sample with 75% RA showed a
porosity of 1.97%, the same tendency in the physical, mechanical and
5
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Table 6
ANOVA of the physical properties.
Property Source of variation SS DF MS F-test p-value Significance

Porosity RA (%) 7.937 3 2.6458 22.435 0.000000 Yes

Error 0.943 8 0.1179
Absorption by immersion RA (%) 2.980 3 0.9933 39.973 0.000000 Yes
Error 0.1988 8 0.0248
Specific gravity RA (%) 0.10257 3 0.03419 512.8 0.000000 Yes
Error 0.00053 8 0.00007

SS = sum of squares; DF = degrees of freedom; MS = mean squares.

Fig. 4. Specific gravity, water absorption, and NA and RA concrete porosity.

Table 7
ANOVA for the compressive strength and the elastic modulus.
Response Source of variation SS DF MS F-test p-value Significancy

Compressive strength Age 956.3 5 191.3 72.83 0.000000 Yes

RA (%) 1780.9 3 593.6 226.05 0.000000 Yes
Age × RA (%) 124.0 15 8.3 3.15 0.008322 Yes
Error 231.1 88 2.6
Elastic modulus Age 956.3 5 191.3 72.83 0.00000 Yes
RA (%) 1780.9 3 593.6 226.05 0.00000 Yes
Age × RA (%) 124.0 15 8.3 3.15 0.00040 Yes
Error 231.1 88 2.6

SS = sum of squares; DF = degrees of freedom; MS = mean squares.

carbonation properties. In addition, the sample with 75% RA also pre­
sented bigger pores and more scattered along the sample. The same
results were found by Da Silva and Andrade [65] and Rashad [66].
3.4. Carbonation depth
The carbonation depth of NA and RA concretes are presented in
Fig. 8(a). Fig. 8(b) shows an example of linear adjustment to Tuutti’s
Equation to determine the carbonation coefficient (k), and Fig. 8(c) the k
values for all evaluated concretes. In the same way, as observed in the
mechanical and physical properties, the increase in RA replacement also
increases the carbonation depth. The 75% RA concrete was the one with
a faster carbonation rate. With 180 days, the 75% RA presented
carbonation 56% higher than the reference concrete.
These results are due to the high permeability and porosity of con­
crete with RA, considering the interconnection between the pore
structures – for both new-mortar and old-mortar. In this way, CO2 finds a
preferable path for diffusion. This tendency is also presented in several
other papers in the literature [59]. The k factor follows the trend for the
fast carbonation rate with the increase in RA replacement level.
Compared to the reference concrete, the RA incorporation increased the
k by 15.0% (25% RA), 60.4% (50% RA), and 75.7% (75% RA). Besides
physical effects, the recycled aggregate has carbonatable material since
the aggregate is also made with cementitious materials.
Moreover, the RA has 35% of ceramic materials in their composition,
which may present some pozzolanic activity and reduce the alkaline
reserve of concrete, contributing to the advancement of carbonation
depth [67]. All aspects discussed can promote the acceleration of the
carbonation process of RA concretes. This behavior follows the logic
observed by Leeman and Moro [68] and Wang et al. [69] the differences
presented in the literature for the same procedure happen due to several
factors influencing the carbonation process, such as cement type, tem­
perature, exposure environment, humidity, and CO2 concentration [70].
However, for uses with no risk of corrosion of the reinforcement, the
greater depth of carbonation is beneficial, as it reduces the porosity of
the matrix and fixes carbon, which is desirable from the point of view of

6
T.L.P. Ortolan et al.
Fig. 5. Mechanical Properties a) Compressive strength b) Elastic modulus.
durability and sustainability [71]. Due to AR’s higher porosity and
chemical composition, cement-based materials produced with this
aggregate fix more carbon than concrete with natural aggregates [38].
3.5. Chloride ion penetration
The ANOVA for the chloride ion penetration is presented in Table 8
for all the parameters that can influence the process.
For the sources of variation analyzed, the most significant, according
to the F-test, were depth, age, and RA%. Following the ANOVA, the
profile was constructed with the adjusted values, made by non-linear
regression by Fick’s Second Law. The profiles for chloride ion penetra­
tion are presented in Fig. 9. Overall, there is an increase in chloride
7
Construction and Building Materials 404 (2023) 133267
concentration in the profiles over time. However, some behaviors con­
trary to this trend can also be observed (e.g., profiles at 112 days). It is
important to consider certain limitations of the technique for deter­
mining chloride concentration. For instance, precision in sampling at
different depths, equipment detection limits for chloride concentration,
and the heterogeneity of concrete and RA can account for the observed
variations. In this regard, it is essential to acknowledge that any test
inherently carries some variability, which may help explain these de­
viations from the expected behavior.
It can be observed that the increase in the RA replacement level also
increases the chloride penetration. For example, for the 2.5 cm depth at
140 days, the reference concrete presented 0.06% chloride concentra­
tion; however, for the sample 75% RA, the value is 0.31% higher for the
T.L.P. Ortolan et al.
Fig. 6. Reference concrete: Reconstructed image (a); Concrete pores (b).
Fig. 7. 75% RA concrete: Reconstructed image (a); Concrete pores (b).
same age. This tendency is explained by the higher porosity of RA
concrete compared to the reference, allowing the chloride to penetrate
easily. Fjendbo et al. [72] performed a similar experiment and could
observe the direct influence of porosity in chloride penetration.
Another point of interest is the difference in chloride content
observed in the first centimeter compared with concretes with low RA
content (25% RA). The low permeability and porosity make it difficult
for the chloride to penetrate. Beyond that, the lines keep getting closer
with the depth advance, probably due to the tendency to decrease the
diffusion coefficient. The time variable reduces the penetration because
the cement keeps hydrating, decreasing permeability and porosity [73].
Ann, Ahn and Ryou [73] explained that some hydration products react
with free chloride ions, forming Friedel Salt, contributing to the
decrease of chloride penetration rate.
The behavior of Cs and D in time was adjusted based on Equations (4)
and (5) to verify the evolution of the parameters for concretes investi­
gated, whose results are presented in Fig. 10.
The continuous decrease in the D coefficient (Fig. 10(a)) can be
observed regardless of the aggregate type (NA or RA). This can be
attributed to the constant hydration process and the subsequent pore
refinement, promoting low permeability, which difficult chloride ion
penetration. The same behavior has been found by many authors in the
literature [74,75]. Additionally, one can note that the corrosion process
in concrete is initiated by the penetration of only free chlorides that are
8
Construction and Building Materials 404 (2023) 133267
dissolved in the pore solution [76]. Therefore, the chloride can react
with the cement constituents (e.g., tricalcium aluminate), and this
binding mechanism decreases the amount of free chloride ions, which
leads to a reduction in the rate of chloride ionic transportation within
concrete [77].
Considering the RA replacement content, the diffusibility of chloride
ions in the cement matrix increases with replacement content, as pre­
sented in several investigations [78,79]. For concretes with 75% RA the
diffusion coefficient was 4.31 cm2/year, three times higher than the
reference concrete (1.53 cm2/year). This trend is consistent with RA
concretes’ higher porosity and lower compressive strength. Zhang and
Zhao [80] explained this behavior by analyzing the transition zone in­
fluence on the mechanical properties and diffusion characteristics of
concrete made with recycled aggregates. The authors verified that the
increase in the RA replacement level promoted the transition zone
thickening. Amorim Junior et al. [25] also verified the same behavior for
concretes with w/c ratios of 0.35, 0.45, and 0.55. The authors also
verified a 22% and 40% decrease in the service life for 50% and 100%
replacements. However, it is necessary to note that the effects promoted
by replacing NA for RA are more evident for high w/c ratios that present
a more permeable matrix. Considering concretes with low w/c ratios,
the chloride penetration trend is more difficult due to the microstruc­
tural densification. Zhang and Zhao[80] explained this behavior by
analyzing the transition zone influence on the mechanical properties
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Fig. 8. Progression of carbonation depth over time (a), an example of adjustment to obtain k for reference concrete (b) and k values for all evaluated concretes (c).

Table 8
ANOVA for the chloride ion penetration.
Source of variation SS DF MS F-test p-value Significancy

Age 2.65370 4 0.66343 112.808 0.000000 Yes

RA (%) 0.07305 3 0.02435 4.141 0.008227 Yes
Depth 50.28353 4 12.57088 2137.527 0.000000 Yes
Age × RA (%) 0.28065 12 0.02339 3.977 0.000051 Yes
Age × Depth 2.51238 16 0.15702 26.700 0.000000 Yes
RA (%) × Depth 0.61372 12 0.05114 8.696 0.000000 Yes
Age × RA (%) × Depth 0.46582 48 0.00970 1.650 0.018338 Yes
Error 0.58810 100 0.00588

SS = sum of squares; DF = degrees of freedom; MS = mean squares.

and diffusion characteristics of concrete made with RA. The authors
verified that the increase in the RA replacement level promoted the
transition zone thickening[25]. Similarly, Villagrán-Zaccardi et al. [81]
also reported that the w/c ratio is more significant on concrete chloride
ingress than the aggregate porosity.
Regarding the Cs in Fig. 10(b), the literature can observe a growth
pattern concerning concretes with NA and RA [78,79,82]. For instance,
the Cs increased from approximately 1.76 % (28 days) to 2.76% (140
days) for NA concrete. However, the increase in RA replacement level
minimizes the chloride on the concretes’ surface. This happens because
the low diffusion rate increases the chloride amount in the concrete
matrix. Silvestro et al. [83] observed the same process and concluded
that the Cs are higher in less permeable concretes. There is a combined
tendency with Cs and D because the hydration process and the perme­
ability make the matrix denser, decreasing D. Otherwise, the Cs are
higher because chloride ions present some difficulty increasing and
accumulating on the surface. According to the F-test shown in ANOVA
results (Table 8), the chloride penetration is more influenced by the age
of concretes (F-test = 112.08) than RA content (F-test = 4.14), that is,
the microstructural characteristics of first deeper (<5 cm) has signifi­
cance in these phenomena. Besides, it can be noted that in this area, the
number of hydrated products in the matrix is more evident because the
coarse aggregates (NA and RA) generally tend to be located deeper from
the concrete surface, explained by the influence found in the ANOVA
test. The same tendency was presented in chloride ion penetration
profiles in Fjendbo et al. [72] investigation.
Generally, it must be observed that there is a synergic effect of Cs(t)
and D(t) in chloride penetration. However, considering conventional
concretes (e.g., w/c = 0.50, resulting in a compressive strength equal to
30 MPa at 28 days), the increase of Cs(t) tends to be more significant
than the decrease of D(t) for the same age.
3.6. Chloride service life prediction
The Brazilian and international standards performed the design
service life prediction to compare the concrete’s performance. It is
important to note that this parameter is related to the time for the
despassivation of reinforcement, considering only the initiation period.
This time is fixed in 50 years by most of the normalization and codes of
practice, and this value will represent the service life in the present
work. Two scenarios were studied to estimate the service life of con­
cretes with RA: the first used Eq. (5) to consider the increase of Cs(t) until
the 50-year mark (Fig. 11). The second analyzed the growth of Cs until
time t = 10 years (Fig. 12), and it is assumed that the value of Cs (t)
remained constant.
According to Andrade et al. [84], the values of Cs in concretes
exposed to the marine environment become constant after 10 years of
exposure. Tang [85] analyzed data collected in 10 years of exposure and
concluded that, in general, the Cs grow until the 5th year. Lee and
Chisolm [86] concluded that concretes with 31 to 69.5 MPa of

9
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Fig. 9. Chloride profiles for concretes with RA.

Fig. 10. Chloride diffusion coefficient (a) and superficial concentration (b) for concretes with NA and RA.

compressive strength at 28 days presented a fast stabilization of Cs after defined that Eq. (5) had a good agreement to predict the evaluate the Cs
5 years of marine environmental exposure. Meira et al. [79] evaluated dependency along the exposure time. Similarly, Eq. 6 simulated the D
concretes for 12 years and concluded that the results varied at first ages, decrease in time for all concretes investigated. This dependency is sig­
but after 6 years, the growth rate was negligible. In this way, it was nificant to make service life prediction values more accurate due to the

10
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Fig. 11. Service life prediction for concretes analyzed considering the Cs growth. a) Without surface treatment; b) System A; c) System B.

Fig. 12. Service life prediction for concretes analyzed considering Cs stabilization after the 10th year. a) Without surface treatment; b) System A; c) System B.

previous restrictions regarding using the 2nd Fick’s Law.
With the modification of 2nd Fick’s Law – including the variation of
Cs(t) and D(t) – it was possible to predict the depth related to critical
chloride ion concentration (Ccr = 0.4%) for concretes with NA and RA.
Besides, different scenarios were investigated to verify the effect of
surface protection systems on chloride penetration. In this way, Fig. 11
shows the service life prediction of NA and RA concretes adopting a Cs
growth and different surface treatments, being: (a) without surface
treatment, (b) application of a silane/siloxane dispersed in a solvent,
and (c) an acrylic dispersed in a solvent (Table 5). Similar results
considering the Cs stabilization after 10 years of exposure and different
treatments are presented in Fig. 12. It can be observed that RA incor­
poration progressively increased the advance of Ccr. Nevertheless, from
replacement content higher than 50%, no expressive increases were
observed for values found. For instance, considering concretes without
surface treatment (Fig. 13(a)), the critical chloride depth predicted after

11
T.L.P. Ortolan et al. Construction and Building Materials 404 (2023) 133267

Table 9 for Cs and D to 50 years for 2nd Fick’s Law (Eq. (4) and (5)), and the
Depth of critical chloride concentration (Ccr) = 0.4% in concretes for t = 50 effect of surface treatment for estimating the service life of concretes
years. with RA, as presented in Table 9.
Concrete Protective Depth of critical chloride Difference The concrete is generally protective against chloride penetration
layer concentration = 0.4% (cm) (%) when delivered on time and has surface protection. However, for con­
REF – 3.33 – cretes with 50% and 75% RA and without surface protection, the rein­
System A 1.85 ↓44.4 forcement can still be protected against chloride penetration with covers
System B 1.66 ↓50.1 of 9.02 and 9.90 cm up to 50 years. These cover values are the only ones
25% 5.56
– –
that do not meet the requirements of the Brazilian and most interna­
System A 3.09 ↓44.4
System B 2.78 ↓50.0 tional standards [88,89].
50% – 9.02 –
System A 5.02 ↓44.3 3.7. Relationship between mechanical and durability parameters
System B 4.51 ↓50.0
75% – 9.90 –
System A 5.51 ↓44.3
Fig. 13 shows the relationship between the physical (porosity), me­
System B 4.95 ↓50.0 chanical (compressive strength and elastic modulus), and durability
properties (diffusion coefficients for carbonation and chloride ingress)
concerned concretes with RA for 28 days. The presence of RA influences
50 years was 4.0 cm (Reference), 6.6 cm (25% RA), 9.9 cm (50% RA), all properties investigated, as discussed in previous sections. The worst
and 10.9 cm (75% RA). Thus, these values represent increases in Ccr situation is related to a 75% replacement level due to their influence on
depth of up to 173% compared to reference concrete. microstructural characteristics.
The increase in the RA replacement level can highlight the decrease Although concretes with RA present lower behavior than concretes
in the design service life prediction. The same tendency was observed by with MA, they can be used in structural elements with low-stress de­
Stambaugh et al. [27] and Neves and Brito [87], which authors inves­ mands, such as slabs, secondary beams, and columns on upper floors,
tigated the influence of five RA contents (20%, 30%, 50%, 70%, and since they meet the requirements established by the structural project.
100%) and verified the reduction of service life with the high RA levels. Thus, the proportioning of the materials can be adapted to obtain
However, the authors conclude that RA can be applied for zones with adequate characteristics for specific purposes.
lower aggressive environments with low replacement levels (until 20%).
Another point to be observed is the difference between the two 4. Conclusions
scenarios applied. For the reference concrete, the time necessary to
achieve the corrosion process is 22 years (in the first scenario) for 48 The study assessed different replacement contents of NA with RA
years (in the second). Similar results were found by Lee and Chisolm concerning mechanical properties, accelerated carbonation, and chlo­
[86], which showed the Cs influence in the service life prediction. ride profile. Additionally, the concretes’ service life prediction analysis
Regarding the reduction in D associated with surface treatment, it was conducted based on Fick’s Second Law, considering (i) stabilization
can be observed that this is an effective approach to increase the service of surface chloride concentration and (ii) decrease in the diffusion co­
life of RA concretes. As shown in Fig. 13, after 50 years, applying an efficient over time. Some conclusions can be made considering all
acrylic treatment dispersed in a solvent reduced the critical chloride properties analyzed:
depth from 9.9 cm (without treatment) to 4.9 cm (System B) for 75% RA
concrete. A similar trend was observed for the other RA contents eval­ • The incorporation of RA increased the porosity and water absorption
uated. Overall, a reduction of approximately 50% on the critical chloride of the concretes by up to 28.0% and 43.0%, respectively. This can be
concentration depth was estimated for System B (acrylic-based treat­ attributed to recycled aggregate’s lower specific gravity and higher
ment) regardless of the exposure time, RA content, and Cs assumptions water absorption.
(growth or stabilization). • A progressive decrease in the compressive strength of concretes was
This information is very important, considering the aggregate type observed with an increase in the replacement content of natural
and composition, the modeling behavior considering the time variations aggregate (NA) by recycled aggregate (RA), regardless of the age
evaluated. The values reached reductions of around 30% (75% RA)
lower than the reference concrete, also assigned to the previously
mentioned aspects.
• The reductions in the modulus of elasticity of concretes with RA are
consistent with the recycled aggregates’ higher porosity than NA.
• The RA also promoted a high carbonation rate: the higher porosity
and permeability facilitated the carbon penetration within the con­
crete matrix. However, other factors like the chemical composition of
RA also contributed to the acceleration of the carbon dioxide
entrance. The 75% RA concrete had a carbonation rate of 210 days,
2.2 times higher than the reference concrete.
• For the chloride ion penetration, the same behavior has been
observed. RA incorporation increased the critical chloride concen­
tration by up to 173% concerning the reference concrete. Never­
theless, it is estimated that applying a surface treatment can reduce
the critical concentration of chlorides by up to 50% for the concretes
evaluated in this study (RA and NA).

Durability studies of RA concrete are essential for consolidating this

aggregate application. This study brought significant contributions
Fig. 13. Relationship between compressive strength, elastic modulus, porosity, concerning carbonation and chloride-induced corrosion. Initially, the
diffusion coefficient and carbonation coefficient. importance of stabilizing the surface concentration and the diffusion

12
T.L.P. Ortolan et al.
coefficient for a realistic service life prediction is verified. In addition,
the work showed that surface treatments could be a good approach to
minimize the negative effect of RA incorporation on the durability of
concretes.
CRediT authorship contribution statement
Tiago Luis Possebon Ortolan: Methodology, Writing. Pietra Mo­
raes Borges: Writing – review & editing. Laura Silvestro: Writing –
review & editing. Sérgio Roberto da Silva: Methodology, editing and
review. Edna Possan: Writing – review & editing. Jairo José de Oli­
veira Andrade: Conceptualization, Supervision, Writing – review &
editing, Funding acquisition.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgments
This study was financed in part by the Coordenação de Aperfeiçoa­
mento de Pessoal de Nível Superior – Brasil (CAPES) – Finance Code 001
to T. L. P. Ortolan and P. M. Borges. Professor J. J. O. Andrade is grateful
for to support of National Council for Scientific and Technological
Development (CNPq), grant 408827/2023-8. The authors are very
thankful to Professor A. B. Masuero from NORIE/UFRGS and the labo­
ratory staff of PUCRS, J. E. Cruz, and D. T. Rodrighiero.
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