Construction and Building Materials 159 (2018) 261–268

Contents lists available at ScienceDirect

Construction and Building Materials

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

Assessment of the durability of grout submitted to accelerated

carbonation test
Roseli Oliveira Guedes Martins a, Rita de Cássia S. Sant’Ana Alvarenga a, Leonardo Gonçalves Pedroti a,
André Fernando de Oliveira b, Beatryz Cardoso Mendes a,⇑, Afonso Rangel Garcez de Azevedo c
a
UFV – Federal University of Viçosa, DEC – Civil Engineering Department, Av. Peter Rolfs, s/n, Campus Universitário, 36570-000 Viçosa, Brazil
b
UFV – Federal University of Viçosa, DEQ – Chemical Department, Av. Peter Rolfs, s/n, Campus Universitário, 36570-000 Viçosa, Brazil
c
UENF – State University of the Northern Rio de Janeiro, LECIV – Civil Engineering Laboratory, Av. Alberto Lamego, 2000, 28013-602 Campos dos Goytacazes, Brazil

h i g h l i g h t s

The advance of the carbonation front decreases with the higher compressive strength.

Spacers must be used to assure the minimum steel cover recommended by the standards.

The useful life of the grout is strongly related with its compressive strength.

It’s necessary to check the durability of structural mansory concerning carbonation.

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

Article history: Durability and useful life of the structural concrete are related to the environmental conditions and
Received 28 June 2017 degrading factors present in the environment. One of most concerning aggressive agents in the civil con-
Received in revised form 19 October 2017 struction industry is carbon dioxide that penetrates into the pores of the concrete reacting with the inter-
Accepted 24 October 2017
stitial hydrates reducing its pH, promoting depassivation of the steel armours inside the concrete, thus
Available online 4 November 2017
enabling to start the corrosion process. This paper produced grout proof-bodies, concretes with high flu-
idity used to fill the blocks in structural masonry, with different resistance to compression: 15 MPa,
Keywords:
20 MPa, 25 MPa. The specimens were submitted to a carbonation front in an accelerated chamber under
Carbonation
Grout
controlled humidity, temperature and carbon dioxide. A numerical model was used aiming to estimate
Durability the forecast of the useful life by making a comparison of the values forecasted by the Brazilian and inter-
national performance rules. It was observed that the 15 MPa grout has a useful life forecast lower than
that recommended by the standard, around 60% lower, while the 20 MPa and 25 MPa grout presented
a satisfactory useful life. Hence, it was certified the importance of controlling the grout resistance and
coverage in structural masonry works as a form to assure the desired durability to the structure.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction explored the relationship between urbanization, one of the most

The emission of carbon dioxide in the atmosphere of the Earth is
an environmental issue of great concern, since from it, it may result
a changing in the climate that will significantly affect the human
life in the planet. Further to affecting life on Earth, the emission
of CO2 also acts on the durability and the useful life of the struc-
tures and constructions produced in reinforced concrete.
For Sheng and Guo [1], the emissions of carbon dioxide gener-
ated by several human activities have increased along decades
regarded the main factor for the global warming. Wang et al. [2]
⇑ Corresponding author.
E-mail address: beatryz.mendes@ufv.br (B.C. Mendes).
plausible markers for the economic development and the demo-
graphic structure along with the emission of carbon dioxide.
According to Villain et al. [3], in the reinforced concrete, the
steel armour is physical and chemically protected against corro-
sion by the surrounding concrete. The interstitial solution of the
pores constitutes a highly alkaline environment where the bars
are passivated. When the carbon dioxide (CO2) in the atmosphere
penetrates into the pores of the concrete, it is dissolved in the
interstitial solution, thus modifying the chemical balances
between the solution and the hydrates, resulting in the carbona-
tion phenomenon.
Jung et al. [4] and Torgal et al. [5] state that the carbonation of
the concrete is one of the main factors affecting the durability of

https://doi.org/10.1016/j.conbuildmat.2017.10.111
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
262 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268
the structures and the major cause for their deterioration. Lo et al.
[6] point out that such process interferes directly in the mechanical
resistance of the reinforced concrete, once it contributes for the
corrosion of the armours inside it.
Corrosion of the armours is a major issue in the maintenance of
the structural integrity of the constructions [7–9], considered by
many researchers as the most frequent issue found in reinforced
concrete structures. In many cases, constructions must be repaired
or reconstructed in a few decades, causing environmental
problems due to the waste generation besides of technical-
economical issues [10].
Both the performance and the useful life of the constructions
have become an increasing concern to civil construction companies
and consumers. Consequently, such subject has also awakened a
lot of interest by part of the researchers in that area. According
to Park [10], the cost of the maintenance in relation to the total
investment in the execution of a building has grown in the last
years. Some of the major issues approached are the early degrada-
tion of newly built constructions and the recovery of structures
presenting pathologies still during the execution.
In order to guide and foster improvements in the execution of
the engineering and architectural projects both in Brazil and
abroad, it has been created normative documentation related to
the construction performance and durability. It may be mentioned
the 13823 ISO: ‘‘General principles on the design of structures for
durability” [11], and ISO 2394: ‘‘General principles on reliability
for structures” [12]; the American rule ACI 318 – 14: ‘‘Building
Code Requirements for Structural Concrete” [13]; Eurocode 2:
Design of structures in concrete – Part 1.1: General Rules and
Building Rules [14], in force in Europe; and Brazilian ABNT NBR
15575-1 rule: Residential Building – Performance [15].
Those standards set the minimum performance parameters
used in constructive systems, for habitational buildings as well in
such extent as to comply with the requirements and demands of
users along the housing cycle of life.
The forecast of the advancement of the carbonation front and
the execution of the accelerated test are recommended as methods
to assess the durability of the structural systems in the 15575-2
ABNT NBR [16]. The 13823 ISO [11] also encompasses the determi-
nation of the useful life of the structures in reinforced concrete
through the carbonation-induced corrosion.
According to Lo et al. [6], the natural carbonation of the concrete
is a chemical reaction between the carbon dioxide (CO2) in the air
and hydration products in the concrete cement. The carbon dioxide
in the atmosphere is dissolved in the water of the pores, producing a
poor carbonic acid (Eq. (1)), which is dissociated (Eqs. (2) and (3))
reacting with the calcium hydroxide (Eqs. (4) and (5)), and later
with the calcium silicate hydrates (Eq. (6)), resulting in the forma-
tion of water and calcium carbonate precipitation (CaCO3), conse-
quently reducing the pH level of the concrete [17].
CO2 ðgÞ þ H2 OðlÞH2 CO3 ðaqÞ
H2 CO3 ðaqÞHþ ðaqÞ þ HCO3 ðaqÞ
HCO3 ðaqÞHþ ðaqÞ þ CO2
3 ðaqÞ
Caþ ðaqÞ þ H2 OðlÞCaOHþ ðaqÞ þ Hþ ðaqÞ
CaðOHÞ2 ðsÞ þ H2 CO3 ðaqÞCaCO3 ðsÞ þ 2 H2 OðlÞ
CaSiO3 :ðg  1ÞH2 O þ H2 CO3 ðaqÞCaCO3 ðsÞ þ SiO2 :gH2 O
In general, the cement present in the concrete is hydrated to
produce an alkali, Ca(OH)2, in the solution inside the pores,
providing a chemical protection to the steel against corrosion. That
chemical protection provided to the steel is performed by a protec-
tive oxide film formed on its surface in an environment with pH
around 13 [18].
Cui et al. [19] expose that whenever the concrete presents pH
values between 8.5 and 9.5, it occurs the depassivation of the steel.
The carbonation phenomenon leads to a decrease in the alkalinity
of the concrete for a lower than 9 pH, thus decreasing its protective
ability and making the steel bars susceptible to corrosion [20].
It is known that the carbonation front of the concrete advances
over time [21,22]. Hence, within the period of useful life foreseen
for a specific structure, it must be avoided that the carbonated
depth reaches the armour, in order to avoid the above mentioned
effects.
Jiang et al. [23] performed the measurement of the carbonation
depth by employing pH markers constituted of a phenolphthalein
solution, as well as Leemann and Moro [24], and Turcry et al.
[25]. It is solution a colorless with a lower than 8.3 pH, and
carmine-red for higher than 9.5 pH, and it may present a varied
pink color in pH values between 8.3 and 9.5.
According to Pan et al. [26], the factors controlling carbonation
are the CO2 diffusivity and the reactivity of the gas with the con-
crete. By its turn, diffusivity depends on the porous structure of
the hardened concrete, its properties and humidity state [21].
Houst and Wittmann [27] complement that information stating
that among the main factors influencing the carbonation speed are:
the water/cement ratio, the cure, the amount and type of the
cement, the carbonic gas concentration, the amount of water, tem-
perature, content of alkalis and cracks.
A form to assess how the carbonation phenomenon affects the
concrete is by applying accelerated tests through the use of
carbonation chambers. Such process is performed by adding higher
CO2 concentrations than the ones found in the atmosphere in envi-
ronments with controlled conditions.
Castellote et al. [28] performed tests in a controlled environ-
ment presenting 65% equilibrium moisture, 22 °C temperature,
and concentration of 0.03% (natural), and 3%, 10% and 100% (accel-
erated). Carbonation was followed-up by the evolution of the mass
gain. They indicated that in the environment with 100% CO2, the
stabilization occurs between the 7th and 40th day, a little earlier
in relation to the environment with concentration of 10% CO2.
Applying a concentration of 3% CO2, the beginning of stabilization
occurs near to the 90th day, and the mass gain increases at a
slower rate. Regarding the carbonation rate, stabilization occurred
more quickly and abruptly under the 100% CO2 concentration.
However, it is not possible to say that carbonation occurred faster,
since the number of measurements was limited.
In recent years, some researchers have used accelerated tests to
assess the durability of concretes, mortars or pastes as to the car-
bonation [29–34]. The authors have applied different controlled
environmental features, and different times of exposition under
such conditions. Bernal et al. [29], Lovato et al. [30] and Morandeau
ð1Þ
et al. [33] adopted relative humidity between 57 and 70%, temper-
ature of 25 °C, and CO2 concentration ranging between 6 and 10%.
ð2Þ Neves et al. [31], Aguiar and Júnior [32], and Duprat et al. [34], on
the other hand, opted for an environment with the same equilib-
ð3Þ rium moisture range, but under temperature of 20 °C and 5%
CO2. Morandeau et al. [33] evaluated the phenomenon in the long
ð4Þ run, with up to 112 days of exposure, while in the others
researches the carbonation was observed in minor ages, from the
ð5Þ 7th day.
Fattuhi [35] performed an accelerated carbonation test to study
the influence of the cure regimen in concrete proof-bodies in rela-
ð6Þ
tion to the 0.70 water/cement submitted to a 100% CO2 concentra-
tion. In his experiments, it was used sampling without wet cure
and sampling water-cured for periods of 1, 3, 5, 7, or 28 days, being
the remaining time air-cured, so each proof-body would complete
 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268
28 days. The results showed that the proof-bodies with cure out-
side water presented an average carbonation front of 25 mm at
the 25th day of the accelerated carbonation.
Calado et al. [36] determined the carbonation advancement by
using the accelerated carbonation test in compacted concretes by
conventional vibration and self-compacting, as a durability marker.
The content of CO2 in a carbonation chamber was 7.5% ± 2.5%, and
the proof-bodies were exposed to such conditions for 22 days. It
was observed that the self-compacting concrete presented 43.8%
as average carbonation in relation to the amount attained by the
conventionally vibrated.
It is noted that there are several papers analyzing the carbona-
tion process in reinformed concrete structures. Nevertheless, there
is no approaching related to such process in the grout, a different
from the conventional concrete.
Grout is a cement mixture, aggregate and water with high
slump used to fill vertical or horizontal voids in masonry to
increase the resistance and enabling the armour adherence. Parse-
kian [37] indicates that the major differences between the grout
and concrete are the high slump (20–25) and the high water/
cement ratio. For him, the grout slump must be adjusted by taking
into account the block absorption, environmental features, temper-
ature and the spaces to be grout.
The purpose of this paper was to assess how the carbonation
phenomenon affects the grout by applying the accelerated carbon-
ation test. With this, attempts were also made to check if the min-
imum coverage of the armours in the structural masonry fixed by
the 15961 ABNT NBR [38] is enough to avoid the early degradation
of the structure. This research showed to be relevant, once such
phenomenon has a negative impact on the durability of that con-
struction system, as well as in the reinforced concrete, resulting
in higher maintenance and repairing expenditures. Hence, the car-
bonation advancement in the grout must be known, as it is respon-
sible by protecting the armours in the structural masonry.
2. Materials and methods
To perform this work, a study of the traces to produce grout was
performed with the characteristic resistances of approximately
15 MPa, 20 MPa, and 25 MPa. In the trace study, it was used an
adaptation of the dosage methodology by the American Concrete
Institute (ACI) and the Portland Cement Institute (PCI), previously
adjusted to the Brazilian conditions by the Brazilian Association
of Portland Cement (ABCP). Traces with lower value of nominal
resistance were selected to check the standards adopted by the
15961-1 ABNT NBR:2011, that recommends in its item 6.1.3 that
for reinformed masonry elements, the resistance to compression
characteristic for the grout must be specified with minimum value
of 15 MPa. The remaining values of grout resistance adopted
(20 MPa and 25 MPa) were selected as they are commonly used
values in the Brazilian civil construction market, and because they
are close to the minimum amount required by the rule. Upon such
conditions, it can be verified the durability and the useful life of a
material often used in the civil construction and also checking if
the limits set by the rule are convenient.
2.1. Grout production
To produce the grout, the following materials were used: CPII E-
32 Portland cement composite; gneiss artificial gravel, graduation
0; natural quartzite sand and multifunctional plastifying additive.
The maximum dimension of the sand used was 4.8 mm; 2.77
fineness modulus; 0.87% powdery material; 2.63 g/cm3 specific
mass (saturated dry surface); 0.80% absorption; 1.07 g/cm3 specific
apparent mass; 1.40 kg/dm3 released unit mass; 1.49 kg/dm3 com-
pacted unit mass.
263
The cement used has a specific mass of 2.95 g/cm3, 402% fine-
ness index, and 34.5 MPa resistance to compression at 28 days.
The gravel of the test had maximum dimension of 12.5 mm;
1.9% powdery material; 3.02 g/cm3 specific mass (saturated dry
surface); 0.20% absorption; 1.52 kg/dm3 released unit mass; 1.63
kg/dm3 compacted unit mass.
For each grout batch produced, it was withdrawn eight (8) sam-
ples, as per Fig. 2. Two proof-bodies from each batch were submit-
ted to compression resistance test following the 5739 ABNT NBR
rule (2007), while another part was put inside the carbonation
chamber. The grout produced presented slump ranging from 19
to 23 cm, providing a good thickening without presenting exuda-
tion. The grout proof-bodies were submitted to carbonation front
test every 3 days, as per item 2.1.2.
The traces in the mass used to produce the grout, as well as
their results of the resistance to compression (fG), are presented
in Table 1.
2.2. Accelerated carbonation test
In order to proceed the reading of the carbonation front devel-
opment, it was used the acid-base phenolphtaleín titrador pro-
duced from a 1% solution dissolved in 96% ethyl alcohol. The
verification of the development of the carbonation front was per-
formed by using the standard presented in Table 4. According to
Cui et al. [19], when the pH of the concrete is lower than 9.5, the
depassivation of the armours begins. Hence, whenever the phe-
nolphtaleín has a light pink color, the pH of the concrete pores is
below 9, and corrosion may appear in the steel bars. Only when
the color is carmine pin, it can be concluded that the environment
remains alkaline.
The carbonation chamber where the test was performed was
mounted to operate in an approximately 100% carbon dioxide con-
centration. The equipment was mounted in the same laboratory,
and the final sketch is shown in Fig. 1. The result of the mounting
is presented in Fig. 2.
The method applied for the CO2 reading is denominated Two
Points Method (M2P) developed by the methodology created by
Adolfo Lutz Institute [39] to set the acidity of beverages. It is a
non-titrimetric potentiometric system consisting of the use of a
buffered solution to check by the difference in the pH certain fea-
tures or substances present in other solution or atmosphere.
The average reading of the concentration along the test was of
85%, reaching 792,281 ppmv. The Brazilian Panel of Climate
Changes [40] indicated a yearly atmospheric concentration in
2016 of 400 ppmv. Thus, the chamber produced an environment
with a CO2 content 1980 times higher with humidity controlled
in the range of 65–80%.
The cylindric proof-bodies of the grout were prepared and sub-
mitted to the accelerated carbonation test over different periods
and with different withdrawing spaces.
In order to check how the development of the carbonation front
occurs over time, the accelerated carbonation test lasted 15 days,
and the proof-bodies were extracted from the chamber every
3 days to make a follow-up of the phenomenon. For this, 12 grout
cylindric proof-bodies were used with 60 mm  100 mm (diame-
ter  height) dimensions. The proof-bodies of the concrete had
their base and top waxed for their faces do not interfere in the side
advancement of the carbonation front.
During the extraction, the proof-bodies were cut according to
the plane shown in Fig. 3 and washed. Next, phenolphtaleín was
applied in the cutting region, in order to check the advancement
of the carbonation front with direction shown in Fig. 4.
The carbonation test was divided in an initial part and the accel-
erated carbonation. The initial one consisted of a test where two
proof-bodies of each grout (15 MPa, 20 MPa, and 25 MPa) were
264 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268

Table 1
Proportions of the grout mixtures used in the tests (cement/sand/gravel/water/additive ratio in mass).

Trace Cement Sand Gravel Water Additive

25 MPa 1 2.042 2.39 0.57 0.005
20 MPa 1 2.333 2.566 0.63 0.005
15 MPa 1 2.928 2.928 0.75 0.005

Table 2
Turning point of the acid-base phenolphtaleín titrador.

Turning point of the acid-base phenolphtaleín titrador

pH
Titrador
7 8 8,5 9 9,5 10 11 12

Phenolphtaleín

Table 3 where xec(t) is the average carbonation depth of the concrete in

Values of slump and resistance to compression attained for the grout.
mm; fc is the resistance specific to the axial compression of the con-
Grout Slump (mm) Resistance to Compression (MPa) crete in MPa; kc is the variable factor related to the type of cement
25 MPa 190 25.0 employed, tabulated; kfc is the variable factor related to the resis-
20 MPa 190 21.0 tance to the axial compression in function of the cement used, tab-
15 MPa 202 16.2 ulated; t is the age of the concrete in years; ad is the content of
pozzolanic addition in the concrete, relative to cement mass; kad
is the variable factor related to the pozzolanic addition of the con-
checked as to the development of the carbonation front out of the crete – active silica, metacauline and rice husk ash – in function
chamber at the day when the other proof-bodies were taken to the of the cement used, tabulated; UR is the average relative humidity;
accelerated carbonation chamber to start the test. kUR is the variable factor related to the relative humidity in function
For the accelerated carbonation test, continuing flows of carbon of the cement used, tabulated; CO2 is the content of CO2 in the
dioxide were performed for 16 min, until the chamber achieve a atmosphere in%; kCO2 is the variable factor related to the content
concentration balance. It was observed an interval of at least 10 of CO2 in the environment in function of the cement used, tabu-
min between injections. Such procedure remained the same at lated; kce is the variable factor related to the exposition to the rain
each extraction of the material tested. in function of the exposition conditions of the structure, tabulated.
The coefficients of the model are tabulated, in function of the
2.3. Mathematical modeling for carbonation depth estimation concrete features, environmental conditions of the accelerated car-
bonation test (CO2 concentration and relative humidity) and struc-
In order to estimate the carbonation depth and predict the use- ture exposition conditions. The values of the coefficients are
ful life of the structure, many empirical mathematical models or available in the Possan et al. [41] work.
complex models have been developed over time [41].
Possan et al. [41] presented a mathematical degradation model
(Eq. (7)) by which is possible to estimate the carbonation depth in 3. Results and discussion
function of the time and attaining a forecast of the useful life in a
concrete structure design. That model was selected because it 3.1. Grout production
has easy to obtain input parameters (resistance to compression,
type of cement and CO2 content in the environment) and a good As previously mentioned, the resistance to compression of the
damage representativity [41]. Besides, it takes into account several grout produced was set and the results attained are presented in
factors that are determinant for the carbonation phenomenon, Table 3.
describing it satisfactorily.
0;5
" 3
!
kfc t kad ad2 3.2. Accelerated carbonation test
xec ðtÞ ¼ kc ð20=f c Þ   exp
20 40 þ f c
! !# The carbonation tests developed in this research were per-
kCO2  CO20;5
kUR  ðUR  0; 58Þ2 formed in two steps. Previously, an initial test was performed to
þ   kce ð7Þ
60 þ f c 100 þ f c decrease the possibility of error. In the main test, the development
of the carbonation front of the grout over time was checked. Upon

Table 4
Carbonation front of the proof-bodies at the starting day of the accelerated test.

Sample Reading of the front (mm) Average (mm)

L1 L2 L3
CP 25.50 4.20 2.93 3.55 3.56
CP 20.62 4.58 5.52 4.11 4.74
CP 15.42 5.72 5.44 3.64 4.93
 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268
Fig. 1. Final sketch of the chamber. (Source: the author).
Fig. 2. Carbonation chambers construed at the lab. (Source: the author).
Fig. 3. Representation of the cutting plan adopted for the specimens. (Source: the
author).
the production data of the grout, the useful life forecast was also
calculated by using a numeric model and its parameters.
That item was produced following the timeline of the results
attained during the tests.
265
Fig. 4. Representation of the carbonation front in the cutting section. (Source: the
author).
3.2.1. Initial advancements tests (EAI)
An initial verification of the advancement of the carbonation
front was performed in the proof-bodies out of the accelerated
carbonation chamber performed on the day the proof-bodies were
placed inside the chamber to start the test. This way, the test had
a previous verification, and it was produced an actual measure-
ment of the development of the accelerated carbonation front,
as such initial measurement can be deemed as the starting point
of the test. Such initial advancement is recorded in Table 4, where
the proof-bodies were numbered by placing first its nominal
resistance, and next the number followed by the lab where the
test was performed. As an example, it was attained the proof-
body CP 25.50 presenting a 25 MPa resistance and at the lab
number 50.
In this paper, the 410-ppm concentration was used as reference
to calculate the useful life forecast for the grout. Such CO2 concen-
tration level in the atmosphere has not been achieved yet, and the
efforts from international entities for it is not achieved are multi-
plying. However, that value was adopted as safety measure by con-
sidering the possibility in the future to attain such concentration.
The forecast for the useful life (VU) of the grout is presented in
the Eq. (7) and its recommendations. The coefficients and data
from the research used in the equation as well as the VU are pre-
sented in Table 5. In order to perform the useful life forecast for
the grout, it was used the minimum coverage value for the
armours recommended by the 15961 ABNT NBR [39], which is
equal to 15 mm (xec).
By observing data in Table 5, it can be verified that the 15 MPa
grout has a useful life of 20 years. Hence, the combination of that
material with any other constructive system whether a concrete
block or a ceramic block, must be assessed. According to the VU
recommendation in the Brazilian Performance Rules for Structural
Systems, the useful life must be higher or equal to 50 years, and
higher or equal to 40 years for sealing masonry. The 2394 ISO
[12] approaching the general security principles also sets a 50
years period as useful life for ordinary constructions and struc-
tures, category comprising structural masonry buildings. In this
case, the grout would enable for the carbonation to reach the steel
armour present inside the concrete after 20 years of its con-
structed, and this would result in the depassivation of the armour,
causing its resistance to the traction to be gradatively reduced and
causing the collapse of the structure.
The 20 MPa grout present a VU result of 42.01 years that alone
would assure only its useful life condition within a sealing system,
266 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268

Table 5
Parameters used and calculation of the useful life for the grout.

Grout xec (mm) kc fc (MPa) kfc kCO2 CO2 (%) kUR UR (%) kce VU (years)
G 15 15.00 22.48 16.33 1.5 15.5 0.041 1300 75 0.65 20.16
G 20 15.00 22.48 21.00 1.5 15.5 0.041 1300 75 0.65 42.01
G 25 15.00 22.48 25.02 1.5 15.5 0.041 1300 75 0.65 69.91

Fig. 5. Development of the carbonation front and CO2 concentration in the carbonation chamber over time.

Fig. 6. Advancement of the carbonation front and carbonation forecast over the
time of the test for 15 MPa resistance to compression grout. Fig. 8. Advancement of the carbonation front and carbonation forecast over the
time of the test for 20 MPa resistance to compression grout.

according to the 15575-2 ABNT NBR [16], bur it would not be

within a short time due to the high carbon dioxide concentration
possible to use that masonry in a structural system.
used to perform the accelerated test. The results are presented in
For the 25 MPa grout, the result of the useful life is 69.91 years,
Fig. 5.
indicating that it can be used without concern to fill both
In this test, it was possible to verify the reduction in the devel-
structural systems and sealing systems assuring the recommended
opment speed of the carbonation front after six days of test, and
durability.
the consequent reduction of the carbon dioxide consumption
It worthwhile to point out that the wall thickness of the con-
inside the chamber. For those 15 Mpa resistance to compression
crete block where the grout is placed was not taken into account,
proof-bodies, it was observed that the total carbonation occurred
since it is very permeable. The carbonation front is spread over it
between the 6th and 9th days of the test.
very quickly; consequently, that thickness of the concrete does
The results presented by Castellote et al. [28], indicate that for a
not cause a significant increase in the useful life forecasted for
100% concentration of CO2 carbonation test, the stabilization of the
the structure.
carbonation occurs between the 7th and the 40th days. This fact
was repeated in the tests presented in this paper.
3.2.2. 15 days test In the accelerated carbonation tests, a forecast of the carbona-
In order to make a detailed assessment of the carbonation front tion front advancement was also performed, based on the param-
in the grout, tests were performed extracting the proof-bodies eters presented in Table 2. The results of the carbonation front

Fig. 7. Development of the carbonation front for 15 Mpa grout.

 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268 267

Fig. 9. Development of the carbonation front for 20 Mpa grout.

It is observed that there is a deceleration in the advancement of

the carbonation front after the six days test, same as it happens to
the 15 MPa of resistance to compression grout.
For the 25 MPa grout, the results are different, as it can be noted
in Figs. 10 and 11.
The 25 MPa resistance to compression grout reached 15 mm
carbonation with a forecast of useful life of 69 years, thus being
kept inside the standards recommended by both the national and
international performance rule for structural systems. It is verified
that there is a deceleration in the advancement of the carbonation
front after the 3-days test, and this may be caused by the clogging
of the pores in the concrete. After the 9-day test, there is another
Fig. 10. Advancement of the carbonation front and carbonation forecast over time
acceleration, and it can be noted in the curve and images.
for the 25 MPa grout resistance to compression. It is pointed out that the greater the resistance to compression
of the concrete, the lesser will be the advancement of the carbon-
ation front, and this was also seen in the works performed by Faus-
for the 15 MPa resistance to compression grout are presented in
tino et al. [43] and Basheer et al. [44]. The proof-bodies with
Fig. 6, and the carbonation images in Fig. 7.
nominal resistance of 15 MPa were already almost completely car-
The forecast of the advancement of the carbonation front over
bonated at the 6-day test, and the 20 MPa and 25 MPa proof-bodies
the years is represented by the dotted lives, and the development
have not been concluded their carbonation after 15 days. One of
of the carbonation front in millimeters is represented by the solid
the possible explanations is that the 15 MPa concrete presents a
lines. It was verified that there is a decrease in the advancement
higher w/c ratio followed by the 20 MPa. Hence, there is a higher
speed of the carbonation front at the day 6 of the test. It was also
amount of water in the macropores of the concrete available to
observed that the 15 MPa grout reached the 15 mm carbonation
react with the carbon dioxide originated from the atmosphere.
– value of the minimum coverage for a reinforced masonry –
Houst and Wittmann [45] also reached the conclusion that the
approximately at 20 years of the forecasted life, that is, an
effective diffusivity of the carbon dioxide in the concrete increases
approximately 60% lower age than the 50 years of useful life,
considerably with the increase in the water/cement ratio.
which is the time for structural systems recommended by the
Thus, during the first days, the carbonation advances with a
15575-2 ABNT NBR [16].
higher acceleration, and after a while, it decelerates due to the
Considering the 2394 ISO [12], the 15 MPa grout does not com-
water consumption in the reactions. Such effect happens in a more
ply as well with the specification of that rule if a 15 mm coverage is
accentuated way to the concrete with lower resistance.
applied.
From the analysis of the results, it can be stated that the mini-
However, the 15673 ISO [42] sets that for structural walls, 30
mum coverage required for the 15961 ABNT NBR [38] is not com-
mm is the minimum coverage, but if that value will be used, it is
patible to the minimum resistance of 15 MPa to comply with the
attained a useful life forecast through the graph of around 100
national and international criteria of useful life of the structure.
years. Hence, if it is assured the minimum coverage mentioned
This marks that the 15 Mpa grout must not be recommended for
in the international rule, the durability criterion as to the useful life
structural masonry constructions, unless it is assured at least 23
will be followed.
mm coverage. Thus, in relation to the 30 mm coverage set by the
Next, the results of the forecast of the advancement of the
15673 ISO [42], the 15 MPa grout could be employed.
carbonation front for the 20 MPa grout (Figs. 8 and 9).
For the grout application even when it is satisfactory as to the
20 Mpa resistance to compression grout reached 15 mm car-
useful life of the building, it must be observed the use of spacers
bonation, with forecast of useful life of 42 years, thus reaching
to truly ensure the 15 mm or higher coverage. It is known that in
the recommended 50 years sealing of the useful life forecasted in
the structural masonry, the breakdown and indication of the spac-
the 2394 ISO [12]. However, its application in sealing masonry is
ers is a seldom-used practice in the designs. Nevertheless, this
allowed according to the 15575-2 ABNT NBR [16]. Following the
research shows the importance to set the use of such devices for
15673 ISO [42], by the use of the 30 mm coverage, the minimum
the minimum coverage be effective in protecting the armour
useful life set by the international rule is out of date.
against corrosion.

Fig. 11. Development of the carbonation front for 25 MPa grout.

268 R.O.G. Martins et al. / Construction and Building Materials 159 (2018) 261–268
4. Conclusions
This paper assessed the grout as to the development of the car-
bonation front. The carbonation test was used as parameter to set
the useful life of that element and then, it was assessed if it com-
plies with the forecasted VU recommended by the performance
rules 15575 ABNT NBR [16] and 2394 ISO [12].
The grout produced at the lab to perform the tests attained the
features for the resistance to compression required both by the
work and fluidity recommended to the material.
The carbonation tests were developed for the grout in two dif-
ferent tests: initial and a 15-day test. In the 15-day test, it was
observed that the advancement of the carbonation front in 15
MPa resistance to compression grout is truly higher than the 20
MPa and 25 MPa grout. This confirms the results for the useful life
through the use of the Possan method that indicates that the mate-
rial produced for the tests with 15 Mpa resistance to compression
is not recommended to be used in sealing or structural masonry.
Still, it can be concluded that the higher the resistance, more
likely will be to achieve a lower advancement of the carbonation
front.
In general, upon the execution of this test, it was possible to
note the importance of using spacers to assure the minimum
15 mm armour coverage recommended by the rule.
The grout used here with minimum resistance to compression
and coverage required by the rules did not comply with the useful
life recommendations from the national and international perfor-
mance rules. It is necessary to perform a detailed study of the grout
formulated with different traces, keeping the same resistance to
compression in order to check if that resistance range can meet
those durability requirements.
Acknowledgments
The authors want to thank the following Brazilian agencies:
CNPq, CAPES and FAPEMIG for their support provided to this
investigation.
References
[1] P. Sheng, X. Guo, The Long-run and short-run impacts of urbanization on
carbon dioxide emissions, Econ. Model. 53 (2016) 208–215.
[2] Y. Wang, L. Chen, J. Kubota, The relationship between urbanization, energy use
and carbon emissions: evidence from a panel of Association of Southeast Asian
Nations (ASEAN) countries, J. Clean. Prod. 112 (2016) 1368–1374.
[3] G. Villain, M. Thiery, G. Platret, Measurement methods of carbonation profiles
in concrete: thermogravimetry, chemical analysis and gammadensimetry,
Cem. Concr. Res. 37 (2007) 1182–1191.
[4] S.H. Jung, M.K. Lee, B.H. Oh, Measurement device and characteristics of
diffusion coefficient of carbon dioxide in concrete, ACI Mater. J. 108 (2011)
589–595.
[5] F.P. Torgal, S. Miraldo, J.A. Labrincha, J. Brito, An overview on concrete
carbonation in the context of eco-efficient construction: evaluation, use of
SCMs and/or RAC, Constr. Build. Mater. 36 (2012) 141–150.
[6] T.Y. Lo, W. Liao, C.K. Wong, W. Tang, Evaluation of carbonation resistance of
paint coated concrete for buildings, Constr. Build. Mater. 107 (2016) 299–306.
[7] M.F. Montemor, M.P. Cunha, M.G. Ferreira, A.M. Simões, Corrosion behaviour of
rebars in fly ash mortar exposed to carbon dioxide and chlorides, Cem. Concr.
Com. 24 (2002) 45–53.
[8] S.K. Roy, K.B. Poh, D.O. Northwood, Durability of concrete – accelerated
carbonation and weathering studies, Build. Environ. 34 (1999) 597–606.
[9] C. Jiang, Q. Huang, X. Gu, Experimental investigation on carbonation in fatigue-
damaged concrete, Cem. Concr. Res. 99 (2017) 38–52.
[10] D.C. Park, Carbonation of concrete in relation to CO2 permeability and
degradation of coatings, Constr. Build. Mater. 22 (2008) 2260–2268.
[11] International Organization for Standardization, ISO 13823 – General principles
on the design of structures for durability, Geneva, Switzerland, 2008.
[12] International Organization for Standardization, ISO 2394 – General principles
on reliability for structures, Geneva, Switzerland, 2008.
[13] American Concrete Institute, ACI 318-14 – Building code requirements for
structural concrete, Farmington Hills, USA, 2014.
[14] European Committee for Standardization, Eurocode 2 – Design of concrete
structures – Part 1.1: General Rules and Rules for Buildings, Brussels, Belgium,
2004.
[15] Brazilian Association of Technical Norms, NBR 15575-1 – Residential buildings
– Performance – Part 1: General Requirements, Rio de Janeiro, Brazil, 2013. (In
Portuguese).
[16] Brazilian Association of Technical Norms, NBR 15575-2 – Residential buildings
– Performance – Part 2: Requirements for structural systems, Rio de Janeiro,
Brazil, 2013. (In Portuguese).
[17] Y. Lo, H.M. Lee, Curing effects on carbonation of concrete using a
phenolphthalein indicator and Fourier-transform infrared spectroscopy,
Build. Environ. 34 (2002) 507–514.
[18] K. Behfarnia, M. Rostami, An assessment on parameters affecting the
carbonation of alkali-activated slag, J. Clean. Prod. 157 (2017) 1–9.
[19] H. Cui, W. Tang, W. Liu, Z. Dong, F. Xing, Experimental study on effects of CO2
concentrations on concrete carbonation and diffusion mechanisms, Constr.
Build. Mater. 93 (2015) 522–527.
[20] A. Steffens, D. Dinkler, H. Ahrens, Modeling carbonation for corrosion risk
prediction of concrete, Cem. Concr. Res. 32 (2002) 935–941.
[21] D.O. McPolin, P.A. Basheer, A.E. Long, K.T. Grattan, T. Sun, New test method to
obtain pH profiles due to carbonation of concretes containing supplementary
cementitious materials, J. Mater. Civ. Eng. 19 (2007) 936–946.
[22] V. Ta, S. Bonnet, T.S. Kiesse, A. Ventura, A new meta-model to calculate
carbonation front depth within concrete structures, Constr. Build. Mater. 129
(2016) 172–181.
[23] L. Jiang, Z. Liu, Y. Ye, Durability of concrete incorporating large volumes of low-
quality fly ash, Cem. Concr. Res. 34 (2004) 1467–1469.
[24] A. Leemann, F. Moro, Carbonation of concrete – the role of CO2 concentration,
relative humidity and CO2 buffer capacity, Mater. Struct. 50 (2017) 30–44.
[25] P. Turcry, L. Oksri-Nelfia, A. Younsi, A. Aït-Mokhtar, Analysis of an accelerated
carbonation test with severe preconditioning, Cem. Concr. Res. 57 (2014)
70–78.
[26] X. Pan, Z. Shi, C. Shi, T.C. Ling, N. Li, A review on surface treatment for concrete
– Part 2: Performance, Constr. Build. Mater. 133 (2017) 81–90.
[27] Y.F. Houst, F.H. Wittmann, Depth profiles of carbonates formed during natural
carbonation, Cem. Concr. Res. 32 (2002) 1923–1930.
[28] M. Castellote, L. Fernandez, C. Andrade, C. Alonso, Chemical changes and phase
analysis of OPC pastes carbonated at different CO2 concentrations, Mater.
Struct. 42 (2009) 515–525.
[29] S.A. Bernal, J.L. Provis, D.G. Brice, A. Kilcullen, P. Duxson, J.S.J. Van Deventer,
Accelerated carbonation testing of alkali-activated binders significantly
underestimates service life: The role of pore solution chemistry, Cem. Concr.
Res. 42 (2012) 1317–1326.
[30] P. Lovato, E. Possan, D.C.C. Dal Molin, J.L.D. Ribeiro, Modeling of mechanical
properties and durability of recycled aggregate concretes, Constr. Build. Mater.
26 (2012) 437–447.
[31] R. Neves, F. Branco, J. Brito, Field assessment of the relationship between
natural and accelerated concrete carbonation resistance, Cem. Concr. Com. 41
(2013) 9–15.
[32] J.B. Aguiar, C. Júnior, Carbonation of surface protected concrete, Constr. Build.
Mater. 49 (2013) 478–483.
[33] A. Morandeau, M. Thiéry, P. Dangla, Investigation of the carbonation
mechanism of CH and C-S-H in terms of kinetics, microstructure changes
and moisture properties, Cem. Concr. Res. 56 (2014) 153–170.
[34] F. Duprat, N.T. Vu, A. Sellier, Accelerated carbonation tests for the probabilistic
prediction of the durability of concrete structures, Constr. Build. Mater. 66
(2014) 597–605.
[35] N.I. Fattuhi, Concrete carbonation as influence by curing regime, Cem. Concr.
Res. 18 (1988) 426–430.
[36] C. Calado, A. Camões, E. Monteiro, P. Helene, B. Barkokébas Jr., Durability
indicators comparison for SCC and CC in tropical coastal environments,
Materials 8 (2015) 1459–1481.
[37] G.A. Parsekian, A.A. Hamid, R.G. Drysdale, Behavior and Dimensioning of
Structural Masonry, first ed., EdUFSCar, Brazil, 2012, 625p. (In Portuguese).
[38] Brazilian Association of Technical Norms, NBR 15691-1 – Structural Mansory –
Concrete blocks – Part 1: Design, Rio de Janeiro, Brazil, 2011. (In Portuguese).
[39] Instituto Adolfo Lutz, Physicochemical methods for food analysis, fourth ed.,
São Paulo, Brazil, 2008, 1020p. (In Portuguese).
[40] Brazilian Panel of Climate Changes, Concentration of CO2 exceeds 400 ppm in
2016. http://www.pbmc.coppe.ufrj.br/es/noticias-es/644-concentracao-de-
co2-passa-400-ppm-em-2016, 2016 (accessed 01.01.2017). (In Portuguese).
[41] E. Possan, E.F. Felix, W.A. Thomaz, CO2 uptake by carbonation of concrete
during life cycle of building structures, J. Build. Rehabil. 7 (2016) 1–9.
[42] International Organization for Standardization, ISO 15673 – Guidelines for the
simplified design of structural reinforced concrete for buildings, Geneva,
Switzerland, 2005.
[43] P. Faustino, C. Chastre, A. Nunes, Carbonation service life modelling of RC
structures for concrete with Portland and blended cements, Cem. Concr. Com.
37 (2013) 171–184.
[44] P.A.M. Basheer, B. Rankin, A.E. Long, D. Russell, Effect of relative humidity and
air permeability on prediction of the rate of carbonation of concrete, Struct.
Build. 146 (2001) 319–326.
[45] Y.F. Houst, F.H. Wittmann, Influence of porosity and water content on the
diffusivity of CO2 and O2 through hydrated cement paste, Cem. Concr. Res. 24
(1994) 1165–1176.