Environ. Sci. Technol.

2010, 44, 3181–3186

steel depassivation. The phenolphthalein indicator technique

Sequestration of CO2 by Concrete is used to measure the carbonation front, which is actually
Carbonation a pH front that differentiates zones with pH below and above
8-9. Closest to the object of this publication, there are some
studies which focus on the amount of CaCO3 formed during
I S A B E L G A L A N , * ,† C A R M E N A N D R A D E , † natural carbonation process. Leber and Blakey (1) used
PEDRO MORA,‡ AND chemical analysis to estimate the carbonation degree in
MIGUEL A. SANJUAN§ mortars and concretes, based on the assumption that all
Eduardo Torroja Institute IETcc-CSIC, Serrano Galvache 4, absorbed CO2 reacts with the lime to form calcium carbonate.
28033 Madrid, Spain, Oficemen, Jose Abascal 53, Madrid Steinour (2) proposed a formula to calculate the amount of
28003, Spain, and IECA, Jose Abascal 53. Madrid 28003, Spain CO2 incorporated by carbonation based on the clinker
composition. Thermogravimetry (TG) and differential ther-
Received November 25, 2009. Revised manuscript received mal analysis (DTA) have been used for both qualitative and
March 3, 2010. Accepted March 3, 2010. quantitative studies of the carbonation phenomenon by some
authors (3-6). Houst and Wittmann (7) used an induction
furnace and an IR analyzer to measure carbonation and
concluded that there is no simple corelation between depth
Carbonation of reinforced concrete is one of the causes of measurements and carbonates profiles. All these authors have
corrosion, but it is also a way to sequester CO2. The characteristics contributed to better delimit the depth of carbonation, and
of the concrete cover should ensure alkaline protection for also to provide information on the amounts of combined
the steel bars but should also be able to combine CO2 to a certain CO2.
depth. This work attempts to advance the knowledge of the There are also some recent publications regarding the
carbon footprint of cement. As it is one of the most commonly CO2 absorption capability of cement based materials from
used materials worldwide, it is very important to assess its U.S. (8, 9), Norway (10) and UK (11). One of the most
exhaustive studies was carried out by a consortium of research
impact on the environment. In order to quantify the capacity
institutes and cement industries from Denmark, Sweden,
of cement based materials to combine CO2 by means of the Norway and Iceland (12-17). This work studies the CO2
reaction with hydrated phases to produce calcium carbonate, absorption capacity of cement based products in these four
Thermogravimetry and the phenolphthalein indicator have been countries throughout their service life and after a process of
used to characterize several cement pastes and concretes demolition and recycling, considering structures of 100 years
exposed to different environments. The combined effect of the of total life, with 70 of service life and 30 of secondary life.
main variables involved in this process is discussed. The The percentages of CO2 absorption given by these authors
moisture content of the concrete seems to be the most influential vary depending on the assumptions taken, the experimental
parameter. measurements on which the studies are based and the
calculations used to obtain the results. As it is very com-
Introduction plicated to extrapolate values and to generalize laboratory
results, the comparison of the results obtained in the different
One of the main problems related to climate change is the studies is very difficult.
greenhouse effect produced by the partial absorption of The main objective of this study was to estimate the
infrared radiation emitted by the Earth by the so-called quantity of CO2 that is reabsorbed into cementitious materials
“greenhouse gases”, including CO2. The United Nations due to the carbonation phenomenon, taking into account
Framework Convention on Climate Change defines “sink” cements’ composition, environments, type of concrete, and
as “any process, activity or mechanism which removes a time. The study was based on Spanish cement, concrete uses
greenhouse gas, an aerosol or a precursor of a greenhouse and applications, and the continental climate in Madrid.
gas from the atmosphere”. As part of the initiatives under-
taken by the cement industry to reduce the greenhouse effect,
this work studies the extent of the CO2 sink effect of concrete Experimental Section
carbonation.
The cements used to fabricate the specimens are given in
Carbonation of concrete takes place when the CO2 from
Table 1. 10 × 10 × 60 mm prismatic paste specimens and
the atmosphere reacts with the alkaline components of
75 × 150 mm cylindrical concrete specimens were produced.
concrete, mainly portlandite, and/or with the CsSsH
Two water/cement ratios (w/c) were used for the mixtures:
(hydrated calcium silicate) gel, resulting in the formation of
0.6 and 0.45. For the specimens with w/c 0.6, cements
CaCO3. The reaction generally leads to a decrease in the pH
numbered 1-12 were used. In addition to the 12 cements
of the aqueous phase of the concrete pores, from very alkaline
selected for the 0.6 w/c specimens three more were added
values greater than 12 to values below 8. If the reaction reaches
for the 0.45 w/c specimens. This explains the ordering of the
the steel reinforcement, its passive layer may disappear,
cements in Table 1, grouped by type of additions. For the
exposing the steel surface to corrosion.
specimens with w/c 0.45, all 15 cement types were used.
Most of the publications related to carbonation are mainly
The concrete mix with 0.6 w/c and 300 kg/m3 is considered
focused on its relationship with rebar corrosion. Their main
representative of concrete used for building works, and the
objective is to measure and predict the progress of the
one with 0.45 w/c and 400 kg/m3 for civil works. The curing
carbonation front and the evolution of corrosion due to the
period was 48 h. The specimens were then dried inside for
26 days. After 28 days the specimens were placed in three
* Corresponding author phone: +34913020440; fax: +34 913020700;
different environmental conditions: outside exposed to the
e-mail: [email protected].
†
Eduardo Torroja Institute IETcc-CSIC. rain, outside sheltered from the rain, and inside, on the
‡
Oficemen. Eduardo Torroja Institute campus in Madrid. As the speci-
§
IECA. mens were put on a grill, all surfaces were exposed to the
10.1021/es903581d  2010 American Chemical Society VOL. 44, NO. 8, 2010 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 3181
Published on Web 03/12/2010
TABLE 1. Cements Selected for the Tests
ref cement clinker % additions CaO % producer origin
1 CEM I 42,5R 95-100 no additions 64 Lafarge-Asland Toledo
2 I 42,5R/ SR 95-100 no additions 63 Uniland Barcelona
14 CEM II/A-L 42,5R 80-94 limestone 62 Cosmos Huelva
3 CEM II/B-LL 32,5N 65-79 limestone 56 Cemex Alicante
4 CEM II/A-M (V-L) 42,5R 80-94 fly ash, limestone 57 Portland-Valderrivas Madrid
5 CEM II/B-M (S-V) 42,5N 65-79 GBFS, fly ash 54 Holcim Almerı́a
6 CEM II/A-P 42,5R 80-94 pozzolan 53 CEISA Las Palmas
7 CEM II/B-P 32,5N 65-79 pozzolan 49 Cemex Toledo
9 CEM II/A-V 42,5R 80-94 fly ash 56 Lemona Vizcaya
10 CEM II/B-V 32,5R 65-79 fly ash 49 Cosmos Córdoba
13 CEM IV/B (V) 32,5N 45-64 fly ash 41 Alfa Santander
8 CEM II/A-S 52,5N 80-94 GBFS 60 Tudela Veguı́n León
15 III/A 42,5N/SR 35-64 GBFS 56 Tudela Veguı́n Oviedo
11 III/B 32,5N/SR 20-34 GBFS 46 Alfa Santander
12 III/C 32,5N/SR/BC 5-19 GBFS 47 Cemex Tarragona

atmosphere. The specimens not sheltered from the rain without additions, 0.5 w/c and 300 kg/m3 were used. The
(Figure 1) were never submerged in water, as rain always thickness of the Hippodrome roof varies from 65 cm in the
washed away. area of the columns to 6 cm at the edges. Samples,
In addition to these specimens made specifically for the approximately 50 mm thick, were taken from both the upper
study, samples from old structures and specimens were taken and the lower part of the roof. The upper part is covered by
and analyzed in order to evaluate the effect of time. Three an asphalt layer added after the construction of the structure.
types of concrete specimens made in 1991, 1999, and 2001 In the pergola, the thickness of the columns also varies from
were selected. The specimens from 1991 were 7 × 7 × 28 cm approximately 30 to 10 cm. The sample taken from the upper
prisms fabricated with 395 kg/m3 and six different experi- part of one of the columns was about 20 mm thick. All
mental mixes: two without additions, two with fly ash, one columns were painted some years after the construction and
with silica fume, and one with fly ash and silica fume. in 1993 some of them were repaired using different methods.
Plasticizers and superplasticizers were used for all mixes. The column chosen for the study was repaired with traditional
The specimens were kept outside sheltered from the rain. mortar.
The specimens from 1999 were 7.5 × 15 cm cylinders After one year of exposure, the carbonation depth, that
fabricated with 400 kg/m3 and microsilica and fly ash is, the depth at which the pH drops below 8-9, was measured
additions as well as superplasticizer. These specimens were in the new specimens by means of phenolphthalein col-
kept inside. The specimens from 2001 were taken from oration. From the uncoloured carbonated part a representa-
concrete used to build a house. A standard mix for building tive sample was taken to perform thermogravimetry (TG)
works was assumed for making the calculations, cement and differential thermal analysis (DTA). These techniques
without additions, 300 kg/m3 and 0.5 w/c. For the first four allow the determination of the carbon dioxide present in the
years these specimens were kept outside exposed to the rain sample from the mass lost in the dissociation of calcium
and the rest of the time sheltered from the rain. carbonate.
Two reinforced concrete structures designed by Eduardo The quantities of calcium carbonate formed in this
Torroja were chosen for taking old samples: the roof of the “carbonated” front may change with depth; the surface may
Zarzuela Hippodrome, built in 1935, and a column from the absorb more CO2 than the inner part. For this study the whole
pergola built in 1951 in the gardens of the Eduardo Torroja “carbonated” part was taken, that is, the average value of
Institute. From the documentation available about concrete CO2 absorption in the zone with pH lower than 8-9 was
in Spain before the seventies and from suggestions from considered. Also, the “noncarbonated” part may absorb CO2
experts in the field, it was assumed that, in both cases, cement even though the pH does not drop below 8, but this
absorption is not taken into account. In this sense the “real”
CO2 absorption might be underestimated.
As the samples’ masses change with time and carbonation
due to the uptake and release of water and the uptake of
CO2, some calculations were done to obtain all values in
percentages of CO2 per gram of cement instead of per gram
of sample. For this, samples were also characterized at the
age of 28 days, and the amount of cement in the sample
(mass that remains after TG calcinations) and the initial
CaCO3 content were taken as reference values. In order to
express the results in CO2 absorbed per mol of CaO available
for carbonation, the CaO content in the different cements
was measured by chemical analysis (Table 1).
For performing TG in the concrete samples, the “mortar”
part was taken, that is, the coarse aggregates were removed
from the samples and the fine aggregate/cement mix
proportions were assumed to perform the corresponding
calculations.
The old specimens were also characterized by the same
two techniques at their corresponding age. It was possible
FIGURE 1. Specimens Outside Not Sheltered from the Rain. to determine the carbonation depth in the old specimens

3182 9 ENVIRONMENTAL SCIENCE & TECHNOLOGY / VOL. 44, NO. 8, 2010

FIGURE 2. Carbonation rates of concrete specimens 0.6 w/c.

FIGURE 3. Carbonation rates of concrete specimens 0.45 w/c.

but not in the case of the old structures because the samples The results clearly show a higher rate of carbonation in
taken were not thick enough to perform the coloration test the concretes made with the mixes considered representative
accurately. The characteristic parameters of environmental of building works (lower cement content) than in the ones
conditions were regularly measured both inside and outside. made with the mixes representative of civil works. This
difference is in some cases as much as double.
Results In general, the specimens that were kept outside sheltered
Environmental Conditions. The relative humidity (RH) from the rain are the ones with the highest carbonation rates,
measured inside varied between 24 and 68% with an average while the ones that were kept inside present the lowest rate.
value of 38%. Outside it varied between 27 and 97% being In this regard, the 0.45 w/c specimens present a more
the average value 57%. The inside temperature was in the homogeneous behavior than those with 0.6 w/c. It is worth
range of 13-25 °C, with an average value of 22 °C, and outside highlighting the increase in carbonation depth with the
0-31 °C, with an average value of 16 °C. The CO2 concentra- percentage of addition within some of the groups of cement
tion measured inside varied between 500 and 850 ppm. types; this effect is indicated by arrows in Figures 2 and 3.
Outside it was almost constant 500 ppm. This high value Concrete specimens 1 and 2 show very similar behavior
compared to the average atmospheric concentration is in the carbonation rate of the front advance in each of the
probably due to the highway which is close to the site where environments, with both w/c ratios. The fact that cement
the specimens were placed. The daily precipitation varied has low C3A and cement 1 has normal C3A content does not
between 0 and 40 mm. appear to have an effect on the carbonation rate.
Carbonation Depths and Rates. A similar behavior in the Regarding the old specimens, most of them presented
carbonation depth with regard to the environment was found rates lower than 3 mm/year1/2, with four of the 1991
in the paste specimens made for the study. In general, specimens not reaching 1 mm/year1/2. The 1999 specimen
specimens outside sheltered from the rain presented maxi- is the one which presents the highest rate, close to 5 mm/
mum depth after 1 year, appearing colorless throughout the year1/2.
tested area. Specimens kept inside also appeared fully The carbonation rates are not easily comparable to the
carbonated throughout the cross section, but in this case data published by some of the authors that have studied the
with very soft pink color, indicating that the pH did not drop natural carbonation phenomenon from the point of view of
below 8. Finally, about half of the specimens kept outside calcium carbonate formation (4, 6, 7), as the environmental
exposed to the rain presented maximum depth colorless, conditions and type of specimens are very different. However
and the other half partial depth with a pink core. it should be noted that none of the rates published by theses
In Figures 2 and 3, the rates of carbonation for the concrete authors exceeds 6.5 mm/year1/2.
specimens with 0.6 and 0.45 w/c in the three exposures are Quantities of Combined CO2. Figures 3 and 4 represent
represented. The rate was calculated with the formula x ) the molar percentages of CO2 absorbed per mol of CaO in
k · t1/2. The specimens are grouped according to type of the “carbonated zone” (indicated by the colorless phenol-
additions, with the reference numbers shown in Table 1. phthalein) after 1 year in the pastes made with 0.6 and 0.45

VOL. 44, NO. 8, 2010 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 3183

FIGURE 4. CO2 quantities absorbed in paste specimens 0.6 w/c.

FIGURE 5. CO2 quantities absorbed in paste specimens 0.45 w/c.

w/c, respectively. These values were measured with TG difference in humidity between the upper and lower parts
analysis, taking the values at 28 days as references. of the roof. The humidity in the upper part might have been
The behavior of the 0.6 w/c specimens (Figure 4) was higher due to its likely exposure to the rain at some points
very homogeneous with regard to the influence of the in time. However, this is only a hypothesis. In general, it is
environment on their CO2 sequestration capacity. The very difficult to give an explanation as we do not know exactly
specimens that absorbed less CO2 were those kept inside, about the repairs, alterations and paintings the old structures
not reaching values higher than 13%. On the contrary, the have undergone throughout their life.
ones that absorbed more CO2 were those that were outside Figure 6 represents all the data of CO2 absorbed as a
exposed to the rain reaching values of absorption of 33 mol function of time collected in this study, both for specimens
of CO2 per 100 mols of CaO in the carbonated zone. The made for the study and for the old ones, as well as for the
specimens that were kept outside sheltered from the rain data collected from the literature. In some cases, as the data
absorbed between 12 and 23% of CO2 per mol of CaO. These are expressed in different units, some calculations and
results demonstrate the great importance of the sample estimations have been made to express the results in the
moisture content in the combination of CO2. same units as the rest of the results in the study.
Regarding the 0.45 w/c specimens (Figure 5) the ones The two horizontal gray and black lines represent the
kept inside were also those that absorbed less CO2, with the maximum possible absorption according to the proposals of
exception of specimen 2 without additions and specimen 4 Steinour (2) and Pade and Guimarares (17), respectively.
with fly ash and limestone. However, the specimens that Since these are different samples and different conditions
absorbed more CO2 were in half of the cases those sheltered the values can not be directly compared, however, it can be
from the rain, and in the other half the ones that were exposed said that in most of the cases absorptions above 50% per mol
to the rain. The behavior of the two groups of concrete of CaO in the carbonated part are not reached.
specimens, w/c 0.6 and 0.45, is similar to the paste specimens
with 0.6 w/c with regard to the environment. In general, with Discussion
few exceptions, the specimens of concrete made with w/c Indicator Parameters and Characterization Techniques.
0.45 absorb less CO2 than the specimens made with w/c 0.6, The depth of carbonation x measured by means of the
being the percentages of CO2 uptake quite similar to those phenolphthalein indicator and the carbonation rate k are
found in the paste specimens. parameters of interest when studying the corrosion of steel
In the old specimens and structures, the quantities reinforced concrete because they help to identify the pH
absorbed varied from zero to 36%. From the group of change front and its evolution with time. However, they do
specimens produced in 1991 three of them did not practically not provide information on the amount of calcium carbonate
absorb CO2 during the exposure time. The other three 17 formed since no general relationship between the depths of
years old specimens did absorb CO2 but did not reach 14% carbonation and the quantities of calcium carbonate formed
of absorption, being the specimens made with fly ash the was found. Trends in the relationship could only be seen
ones that absorbed more CO2. The specimen made in 1999 within groups of samples.
absorbed less than 10% of CO2 per mol of CaO in nine years. The amount of CO2 absorbed is also a key parameter not
The specimens made in 2001 with a building type of concrete only to calculate the ability of cement based materials to
absorbed between 27 and 36% CO2 in seven years. In the reabsorb CO2, but also to model the progress of carbonation.
tested sample of the Pergola, a quantity of 33% of CO2 Using Thermogravimetrical techniques the carbon dioxide
absorbed over about 57 years was measured. The two samples absorbed and combined as calcium carbonate can be
from the Hippodrome absorbed very different amounts of determined. Other techniques should be used to measure
CO2: about 30% in the upper part and 3% in the lower part. other possible minor contributions to CO2 absorption arising
The difference might be explained as a consequence of the from other phases, and more research should be performed

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FIGURE 6. Quantities of CO2 absorbed as a function of time 0-80 years.
in the future in order to complement these data and to avoid Regarding CO2 combined there are very few models or
the underestimation of the CO2 absorption. proposals. The evolution of CO2 combination with time is
Influence of the Exposure Environments. Humidity is not evident. Young samples may have greater uptake than
one of the most influential factors in the advancement of the older ones. In general, the ones studied here do not exceed
carbonation front and in the amount of CO2 combined. In 50% of CO2 absorption (per CaO mol) in the carbonated
general terms, specimens made for the study that were kept zone.
outside sheltered from the rain presented higher carbonation Composition of Concrete. By increasing the amount of
depth after one year than those that were outside not cement in the concrete, both the carbonation depth and the
sheltered. In contrast, the amounts of CO2 absorbed in this amount of CO2 absorbed decrease, being the main cause for
“carbonated” zone were greater in the specimens that were that the decrease in porosity. The fact that the amount of
outside exposed to the rain than in the ones kept outside CO2 decreases as the cement content increases indicates that
sheltered. These differences are attributed to the degree of a decrease in porosity has a higher influence than an increase
water saturation of the pores resulting from the moisture of the amount of carbonatable material.
changes that occur inside the concrete as a consequence of Calculation of CO2 Absorbed. Based on the carbonation
the rain-drying cycles. depth data, the CO2 absorbed in the carbonated zone, the
The amount of CO2 combined in the specimens and the exposed surface of the concrete, and the mix proportions,
carbonation depth reached during the first year of exposure the amount of CO2 absorbed per m3 of concrete in a structure
were considerably lower in the internal environment than in can be calculated.
the external environment. This result indicates that a higher The corresponding CO2 absorbed in the carbonated
concentration of CO2 in the interior does not imply a greater concrete is determined by multiplying the CO2 absorbed
sequestration of CO2 in the range of CO2 concentrations per kg of cement in the carbonated zone by the amount
considered. The other parameters involved, mainly the of cement in the concrete. On the other hand, by
relative humidity, appear to have a greater influence. multiplying the carbonation depth by the relationship
Type of Cement. There are significant differences in the between exposed surface and concrete volume, the
resistance to carbonation (amount combined and carbonated relationship between carbonated concrete volume and
depth) of the different specimens depending on the type of total concrete volume is determined. Finally multiplying
cement used, linked both to the type of additions and to the these two terms, the CO2 absorbed per total concrete
amount of clinker per m3 of concrete. In general, with volume is calculated.
increasing amount of clinker, the amount of CaO increases, The results can also be expressed per ton of cement
that is, material subject to carbonate. When introducing produced taking into account the relationship between
additions to the cement, it is important to take into account cement produced and concrete consumed. To express the
that the water/clinker ratio will increase, but it is also very results per ton of CO2 emitted, the relationship between the
important to know the contribution of the additions to the amount of cement produced and the amount of CO2 emitted
CaO content. in their production should be considered.
By increasing the amount of CaO, the amount of CO2 As there are not enough available data of surfaces exposed
absorbed increases generally and the depth of carbonation to carbonation and as the cement and concrete market is
decreases, being the relationship with depth much more clear continuously changing, the calculations of the CO2 seques-
than the relationship with the combined CO2. Both relation- tration should be done very carefully. Considering the
ships become more evident when considering the groups of carbonated zone as the region where the pH is lower than
additions separately, and also when dividing them by 8-9 may underestimate the real CO2 absorption in the whole
environments. In any case, it is important to note the presence volume, because, as stated before, there might be absorption
of exceptions. as well in the region with higher pH. To obtain more accurate
It can be stated that there is a combined dependence of calculations absorption profiles at all depths in the samples
the type of cement and the environmental conditions on the should be measured in the future, both in front and behind
carbonation. the pH front.
Life Time. There are several models to predict the progress From the data obtained in this study, it can be concluded
of the carbonation front, mostly based on the solution of that the carbonation depth is not a correct indicator of the
Fick’s law. The effectiveness of these models has been amount of sequestered CO2. Regarding the parameters
experimentally tested on numerous occasions. However, it influencing the CO2 sequestration, higher water/cement ratio
is important to be cautious when using them as the constants implies normally higher porosity which, in turn, leads to
of proportionality depend on many factors. higher CO2 absorption. Within groups with the same type of

VOL. 44, NO. 8, 2010 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 3185

additions, the amount of CO2 bound increases with the CaO (7) Houst, Y. F.; Wittmann, F. H. Depth profiles of carbonates formed
content. The big differences between exposure sheltered and during natural carbonation. Cem. Concr. Res. 2002, 32, 1923–
not sheltered from the rain demonstrate that the moisture 1930.
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content of the concrete is a key parameter in the sequestration Dioxide: a Literature Review and Estimation of CO2 Absorption
of CO2 by natural carbonation. In general, while the influence by Portland Cement Concrete, R&D Serial no. 2255; PCA: Chicago,
of the type of cement and the proportion of cement can help IL, 2000.
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Norwegian OPC Concrete; CANMET/ACI International Confer-
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This work was supported by the Spanish Ministry of Science British Cement Association: Camberly, UK, 2007.
and Technology, Oficemen, and CSIC to whom the authors (12) Kjellsen K. O.; Guimaraes M., Nilsson A. The CO2 Balance of
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