Construction Materials Proceedings of the Institution of Civil Engineers

http://dx.doi.org/10.1680/jcoma.17.00015
Improving the properties of recycled Paper 1700015
Received 02/03/2017 Accepted 22/05/2017
concrete aggregates by accelerated
Keywords: concrete technology & manufacture/
carbonation recycling & reuse of materials/sustainability
Zhao, Remond, Damidot, Courard and Michel

ICE Publishing: All rights reserved

Improving the properties of recycled concrete

aggregates by accelerated carbonation
Zengfeng Zhao PhD
Senior researcher, Department of ArGEnCo, GeMMe Building Materials,
Urban and Environment Research Unit, University of Liège, Liège, Belgium
(corresponding author: zengfeng.zhao@ulg.ac.be)
Sébastien Remond PhD
Professor, IMT Lille Douai, Civil and Environmental Engineering
Department, University of Lille, Lille, France
Denis Damidot PhD
Professor, IMT Lille Douai, Civil and Environmental Engineering
Department, University of Lille, Lille, France
Luc Courard PhD
Professor, Department of ArGEnCo, GeMMe Building Materials,
Urban and Environment Research Unit, University of Liège, Liège,
Belgium
Frédéric Michel MSc
Senior researcher, Department of ArGEnCo, GeMMe Building Materials,
Urban and Environment Research Unit, University of Liège, Liège, Belgium

Large amounts of construction and demolition wastes, especially concrete wastes, are generated annually. Until
now, only a small fraction of concrete wastes has been reused as recycled concrete aggregates (RCA) in the
manufacture of mortar and concrete. In order to optimise the use of RCA for new concrete, it is important to improve
the properties of RCA. RCA are mainly composed of an intimate mix of natural aggregates and adherent hardened
cement paste, which has a much larger porosity than natural aggregates. The influence of accelerated carbonation
on the properties of RCA was studied in this work. Original concrete was manufactured and crushed by a jaw crusher
in the laboratory. The different fractions of laboratory-produced RCA were stored in an accelerated carbonation
room. The mass loss, density, porosity and water absorption of the RCA were tested before and after carbonation.
Industrial RCA were also studied for comparison with the laboratory-produced RCA. The results clearly showed that,
after accelerated carbonation, the density of the RCA increased due to the transformation of portlandite into calcite.
The water absorption and porosity of the RCA decreased after carbonation.

1. Introduction
Due to the population growth and the rapid development of
the construction industry, large amounts of construction and
demolition wastes are generated all over the world every year,
and these quantities are expected to increase in the future
(Rao et al., 2007; Sagoe-Crentsil et al., 2001). It is very impor-
tant to recycle these wastes in order to protect the environ-
ment. A minimum of 70% (by weight) of non-hazardous
construction and demolition wastes should be prepared for
reuse or recycled by 2020 according to the waste framework
directive (2008/98/EC) (EU Commission, 2008). Large quan-
tities of natural aggregates are needed for the construction
industry. Until now, only small percentages of concrete wastes
have been reused as recycled concrete aggregates (RCA) in the
manufacture of mortar and concrete (Courard et al., 2010; De
Juan and Gutiérrez, 2009; Hansen, 1986; McNeil and Kang,
2013; Poon et al., 2002; Zhao et al., 2015). In order to opti-
mise the use of RCA for new concrete, it is important to
improve their properties (e.g. water absorption and porosity).
RCA comprise an intimate mix of natural aggregates and har-
dened cement paste. The properties of RCA depend on many
factors such as the original concrete, contaminants, particle
size, crushing method for production, storage conditions and
so on (Etxeberria et al., 2007; Evangelista and de Brito, 2007;
Tam et al., 2008). Hardened cement paste generally presents a
much larger porosity than natural aggregates and therefore the
content and physicochemical properties of hardened cement
paste have a large influence on the properties of RCA (Zhao
et al., 2013, 2015).
Carbonation is a procedure (Reaction I) by which carbon
dioxide (CO2) in the atmosphere penetrates and diffuses through
the pore water and reacts with calcium hydroxide (Ca(OH)2),
producing calcium carbonate (CaCO3) and water (Johannesson
and Utgenannt, 2001; López-Arce et al., 2011). In addition,
hydrated calcium silicate (C–S–H) can also react with carbon
dioxide according to Reaction II (Chang and Chen, 2006).
I: CaðOHÞ2 þ CO2 ! CaCO3 þ H2 O
II: C--S--H þ CO2 ! CaCO3 þ SiO2 :nH2 O
Ngala and Page (1997) investigated the effect of carbonation on
the pore structure and diffusional properties of hydrated cement
pastes. Their results showed that the total porosity for all the
studied pastes reduced after carbonation (Ngala and Page,
1997). However, few studies have been dedicated to the influence
of carbonation on RCA. Apart from the potential benefit on

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 Construction Materials Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel

Table 1. Original concrete composition made in the laboratory (1 m3)

Cement: kg Coarse aggregate: kg Sand: kg Water: kg w/c ratio 90 d compressive strength: MPa

298·8 1138·3 756·4 179·3 0·6 47

the performance of RCA, the carbonation process could also

have the environmental benefit of reducing carbon dioxide emis-
sions, which is a huge international challenge. Pure carbon dioxide out

The possibility of improving the properties of RCA (water absor- Sodium chloride
ption and porosity) by accelerated carbonation was studied. Samples solution

Original concrete was manufactured in the laboratory and

then crushed using a jaw crusher. The different fractions of lab-
oratory-produced RCA were stored in an accelerated carbonation Pure carbon dioxide in

room. The mass loss measured by thermogravimetric analysis

(TGA), density, porosity and water absorption of the RCA were
tested before and after carbonation. Industrial RCA were also
studied for comparison with the laboratory-produced RCA.
Figure 1. Carbonation cell used for RCA

2. Materials and methods

2.1 Materials
2.1.1 Laboratory-manufactured RCA
Original concrete was manufactured for the production of RCA.
Table 1 shows the details of the original concrete composition.
The cement used in this study was a white ordinary Portland
cement (CEM I 52·5 ‘superblanc’) provided by Lafarge.
Crushed calcareous sand and calcareous coarse aggregates
sourced from Tournai (provided by Holcim France Benelux)
were used for production of the original concrete. After 90 d
curing in water, the concrete was crushed in the laboratory
using a jaw crusher with an opening size of 10 mm. After crush-
ing, the RCA were dried in an oven at 105°C. In this study, the Figure 2. Carbonation tested by phenolphthalein solution (left:
focus was on fine RCA (FRCA) (0/5 mm) with the coarser frac- before carbonation; right: after carbonation)
tion of RCA (CRCA) essentially composed of natural aggre-
gates generally possessing properties satisfactory for reuse as phenolphthalein did not turn pink, indicating that carbonation
concrete aggregates. The FRCA were then separated by sieving of the sample was almost complete, at least at their surfaces
into four different granular classes (0/0·63, 0·63/1·25, 1·25/2·5, (Figure 2). All the granular classes of laboratory-manufactured
2·5/5 mm) in order to study the influence of granular class on well-carbonated RCA (denoted RCAl_wc) and laboratory-
the properties of RCA. The four different granular classes of manufactured non-carbonated RCA (denoted RCAl_nc) were
RCA were stored in sealed bags in order to minimise carbona- characterised, including mass loss measured by TGA, density,
tion (considered as non-carbonated RCA). In the following, porosity and water absorption.
each granular class is represented by its average particle size,
corresponding to the average value of the minimal and maximal
particle sizes of the granular class. 2.1.2 Industrial RCA
RCA produced at an industrial recycling centre were also
The four different granular classes of RCA (about 1 kg) were used (denoted RCAi). The RCAi were produced at a recycling
then stored in a pure carbon dioxide carbonation cell at 20°C centre in Louvres (Colas). Only the 0/5 mm fraction of RCAi
(Figure 1). Supersaturated sodium chloride solution was used was studied and this was subdivided into the four granular
to obtain a constant relative humidity of 75%. After 2 weeks classes previously used for the RCA made in the laboratory.
of accelerated carbonation, a solution of phenolphthalein was All the granular classes of industrial RCA were tested for the
used as an indicator to check the carbonation degree. The same properties as the laboratory-manufactured RCA.

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 Construction Materials Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel

2.2 Experimental methods

2.2.1 TGA
1
Representative samples of each granular class were pre-dried in
an oven at a temperature of 105°C. A representative sample
powder was then obtained by grinding the material to a
maximum size of 0·2 mm, and TGA with analysis of the gas
by mass spectrometry (MS) was then carried out (Netzsch
STA449 F3). Heating was conducted in three phases
2
& from ambient temperature to 105°C at a heating rate of
2°C/min
& 30 min at a constant temperature of 105°C
& from 105 to 1100°C at a heating rate of 3°C/min.

2.2.2 Density
For each of the RCA and each granular class, representative
samples were pre-dried in an oven at a temperature of 105°C
3
and then density was measured using a helium pycnometer
(Micromeritics AccuPyc 1330).

2.2.3 Water absorption

The water absorption coefficient (WA) of each granular
class of RCA was measured using IFSTTAR method 78
(IFSTTAR, 2011). Three samples of each granular class of
RCA were measured to obtain the average value. The samples
were saturated for 24 h in water and then the WA was deter-
mined based on the water content in the saturated surface dry
(SSD) state. The aggregates were dried progressively with
different sheets of coloured absorbent paper until no trace of
water could be seen on the paper, and the SSD mass (M1) was
measured. The surface of each sheet of coloured absorbent
paper was wiped carefully with a brush to ensure that no fine
particles remained attached to the paper. In that SSD state,
no moisture remained on the surface of the particles (third
sheet of paper in Figure 3). The aggregates were then dried in
an oven at 105°C to constant mass (M2). The WA of the RCA
was then calculated according to
M1  M2
3: WA ¼  100
M2
2.2.4 Porosity
The 2·5/5 mm fractions of RCAl_nc and RCAl_wc were tested
by mercury intrusion porosimetry (MIP) using a Micromeritics
Autopore IV machine.
3. Results and discussions
3.1 TGA results with analysis of gas by MS
Figures 4 and 5 present the TGA results with analysis of
gas by MS for the 1·25/2·5 mm fraction of RCAl_nc and
Figure 3. Water traces after successive dryings with absorbent
paper (IFSTTAR method)
RCAl_wc. In these figures, the peak at 150–175°C corresponds
to a loss of water in C–S–H. The peak at 450°C corresponds
to the loss of water in portlandite (similar results were reported
by Alarcon-Ruiz et al. (2005) and DeJong and Ulm (2007)).
This peak almost disappeared after carbonation, meaning that
the portlandite had transformed to calcite.
Figures 4 and 5 first show that the loss of carbon dioxide in
uncarbonated samples was negligible at temperatures lower than
600°C. This confirms that, in the uncarbonated samples, the
mass loss between 105 and 600°C (ML105–600) was essentially
due to loss of water. When cement paste is not carbonated, the
peak due to carbon dioxide/carbon monoxide is linked only
to the decomposition of limestone aggregates and is located
between 600 and 900°C. However, when cement paste is carbo-
nated, decarbonation starts earlier (from 500°C). Figure 5 clearly
shows that part of the mass loss between 105 and 600°C was due
to the loss of carbon dioxide.
Figure 6 presents the TGA results with analysis of gas by
MS for the 1·25/2·5 mm fraction of RCAi. A large peak of
mass loss was obtained between 500 and 850°C due to the
loss of carbon dioxide, which suggests that the RCAi contained
calcareous aggregates. Moreover, significant decarbonation
started at 500°C, and the carbon dioxide loss starting from
500°C makes it possible to highlight carbonation of the

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 Construction Materials Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel

100 Change in mass: –2·83% [1·3] 2·0

0
95
1·5 –0·2
90

Current × 10–9: A

DTG: %/min
85
TGA: %

–0·4
Change in mass: –32·07% 1·0
80
Carbon dioxide
–0·6
75
Water
0·5
Carbon
70 monoxide
–0·8
65 0

200 300 400 500 600 700 800 900 1000

Temperature: °C

Figure 4. TGA with gas analysis: RCAl_nc 1·25/2·5 mm. A full-colour version of this figure can be found on the ICE Virtual Library
(www.icevirtuallibrary.com)

Change in mass: –3·73% [1·3]

100 1·6 0
95 1·4
–0·2
90 1·2
Current × 10–9: A –0·4

DTG: %/min
85 1·0
TGA: %

Change in mass: –34·41% –0·6

80 0·8

Carbon dioxide 0·6 –0·8

75
0·4 –1·0
70 Carbon
monoxide
Water 0·2
65 –1·2
0
60
–1·4
200 300 400 500 600 700 800 900 1000
Temperature: °C

Figure 5. TGA with gas analysis: RCAl_wc 1·25/2·5 mm. A full-colour version of this figure can be found on the ICE Virtual Library
(www.icevirtuallibrary.com)

cement paste; this thus shows that the RCAi were partly
carbonated.
Table 2 shows the values of mass loss between 105 and 400°C
(ML105–400), between 400 and 500°C (ML400–500), between 500
and 600°C (ML500–600), between 600 and 700°C (ML600–700)
and between 700 and 1095°C (ML700–1095) based on TGA with
gas analysis. For all the studied RCA, ML105–400, ML400–500,
ML500–600 and ML600–700 increased as the particle size of the
RCA decreased. ML700–1095 corresponds to the content of crys-
tallised calcite in the sample. Therefore, the finer fraction of
RCA contained a higher quantity of portlandite and the finer
fraction of RCA had a larger hardened cement paste content
and a higher porosity compared with the CRCA. After carbo-
nation, ML400–500 decreased, which is due to the transform-
ation of portlandite onto calcite, leading to a smaller loss of
water. ML400–500 corresponds partly to the water bounded by
portlandite (MLH2 O-400500 ) and some decarbonation of amor-
phous calcite (MLCO2 -400500 ). However, at the same time,
ML500–600 and ML600–700 increased after carbonation due to a
significant loss of carbon dioxide between 500 and 700°C. This
suggests that the formation of amorphous carbonation pro-
ducts occurred during the accelerated carbonation tests (as
confirmed by Thiery et al. (2007) and Villain et al. (2007)).

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 Construction Materials Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel

100 Change in mass: –2·50% [1·3] 9·00

0
8·00
–0·1
95 7·00
–0·2
6·00

Current × 10–10: A

DTG: %/min
5·00 –0·3
90
TGA: %

Change in mass: –20·00%

4·00 –0·4

85 Carbon dioxide 3·00 –0·5

Water 2·00 –0·6

[2]
80 1·00
Carbon –0·7
monoxide
0 –0·8
200 300 400 500 600 700 800 900 1000
Temperature: °C

Figure 6. TGA with gas analysis: RCAi 1·25/2·5 mm. A full-colour version of this figure can be found on the ICE Virtual Library
(www.icevirtuallibrary.com)

Table 2. Mass loss based on TGA with gas analysis for all studied RCA
ML105–400 ML400–500 ML500–600 ML600–700 ML700–1095

RCAl_nc 0/0·63 2·04 1·04 0·35 1·59 29·33

RCAl_nc 0·63/1·25 1·81 1·02 0·32 1·37 29·99
RCAl_nc 1·25/2·5 1·53 1·01 0·3 1·22 30·85
RCAl_nc 2·5/5 1·44 0·98 0·29 1·21 31·25
RCAl_wc 0/0·63 1·03 0·88 2·91 3·54 29·39
RCAl_wc 0·63/1·25 0·94 0·8 2·54 3·11 30·74
RCAl_wc 1·25/2·5 0·81 0·69 2·23 2·8 31·63
RCAl_wc 2·5/5 0·68 0·6 1·92 2·49 32·58
RCAi 0/0·63 1·98 0·64 0·72 1·92 13·11
RCAi 0·63/1·25 1·68 0·55 0·57 1·5 17·19
RCAi 1·25/2·5 1·48 0·5 0·52 1·37 18·63
RCAi 2·5/5 1·34 0·47 0·73 1·62 19·28

Table 3. MLH2 O-400500 and MLCO2 -400500 based on TGA with gas analysis
SH2 O SCO2 ML400–500 MLH2 O-400 –500 MLCO2 -400 –500

RCAl_nc 0/0·63 0·50 0 1·04 1·04 0

RCAl_wc 0/0·63 0·03 0·12 0·88 0·07 0·81
RCAi 0/0·63 0·42 0·06 0·64 0·47 0·17

From the curves for gas analysis by MS, the surface areas of
water (SH2 O ) and carbon dioxide (SCO2 ) can be estimated, then
the mass ratio of water can be calculated. Thus MLH2 O-400 –500
can be obtained from
18  S H2 O
4: MLH2 O-400500 ¼ ML400500 
44  S CO2 þ 18  S H2 O
Table 3 shows the calculated results of MLH2 O-400500 and
MLCO2 -400500 for the 0/0·63 mm fraction. As can be seen, the
mass ratio of carbon dioxide in ML400–500 changed as the
carbonation degree changed. For RCAl_nc, ML400–500
was entirely from the water bounded by portlandite. For
RCAl_wc, MLCO2 -400500 was 92% of ML400–500. For RCAi,
MLCO2 -400500 was 26%. As a consequence, the portlandite
content of industrial RCA was between that of the non-
carbonated RCA and well-carbonated RCA.
3.2 Density
Figure 7 shows the variation in density measured by means of
a helium pycnometer as a function of granular class. It shows
that the density of RCA increased as the average particle size

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 Construction Materials
2·62
2·60
2·58
2·56
Density: g/cm3
2·54
2·52
2·50 RCAl_nc
RCAi
2·48
RCAl_wc
2·46 Linear (RCAl_nc)
Linear (RCAl_wc)
2·44
0 1 2 3 4 Fraction of RCA: mm
Average size: mm
Figure 7. Density of all the studied RCA as a function of average
size of the four different granular classes considered (0/0·63,
0·63/1·25, 1·25/2·5, 2·5/5 mm)
increased for all the studied RCA. The density of all fractions
of RCAl_wc was higher than that of RCAl_nc. This is due to
the transformation of portlandite into calcite; indeed, calcite
has a higher density than portlandite. After carbonation, the
slope of the density–average particle size plot of RCAl_wc was
lower than that of RCAl_nc. This can be explained by the fact
that the finer fraction of RCA has a higher hardened cement
paste content, and the density of the latter was increased by
the carbonation. The density of all the fractions of the indus-
trial RCA was higher than that of RCAl_nc. The higher values
of density obtained for the RCAi could be due to carbonation;
however, the composition of the RCA, the density of natural
aggregates and the density of cement paste in the RCA (which
were not known) could also change the density of industrial
RCA.
3.3 Water absorption and porosity
Figure 8 shows the WAs of the four granular fractions of
RCAl_nc and RCAl_wc measured by the IFSTTAR method.
The WAs for all the granular classes of RCAl_wc were signifi-
cantly lower than those obtained for RCAl_nc. This can be
attributed to the reduction of cement paste porosity due to car-
bonation. After carbonation, the WA of RCA decreased by
32·8, 30·9, 31·1 and 25·8% for the 2·5/5, 1·25/2·5, 0·63/1·25 and
0/0·63 mm fractions, respectively. A similar observation was
reported by Grabiec et al. (2012).
The MIP results of RCAl_nc and RCAl_wc show that the
porosity of RCA decreased after carbonation, from 14·1% to
7·8%, and the transformation of portlandite into calcite and
the formation of amorphous carbonation products during
accelerated carbonation tests reduced the porosity of the
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Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel
20
18
16
RCAl_nc RCAl_wc
Water absorption: %
14
12
10
8
6
4
2
0
0/0·63 0·63/1·25 1·25/2·5 2·5/5
Figure 8. Water absorption of RCAl_nc and RCAl_wc measured
by the IFSTTAR method
hardened cement paste, which led to the reduction of WA of
RCA after accelerated carbonation.
4. Conclusions
The possibility of improving the properties of RCA by
accelerated carbonation was studied. Non-carbonated RCA
(RCAl_nc), well-carbonated RCA (RCAl_wc) and industrial
RCA (RCAi) were tested for mass loss (measured by TGA),
density, porosity and water absorption. The main conclusions
obtained are as follows.
& The finer fraction of the RCA contained a higher quantity
of portlandite and had a higher hardened cement paste
content and a higher porosity than the coarser fraction.
After accelerated carbonation, ML400–500 decreased, which
is due to the transformation of portlandite into calcite
leading to a smaller loss of water. At the same time,
ML500–600 and ML600–700 increased after carbonation, due
to a significant loss of carbon dioxide between 500 and
700°C. The formation of amorphous carbonation products
occurred during the accelerated carbonation tests. The
portlandite content of the RCAi was between that of the
RCAl_nc and RCAl_wc.
& The density of all the fractions of RCAl_wc was higher than
that of RCAl_nc. This is due to the transformation of
portlandite into calcite; indeed, calcite has a higher density
than portlandite.
& The WAs obtained for all the granular classes of RCAl_wc
were significantly lower than those obtained for RCAl_nc.
This can be attributed to a reduction in hardened cement
paste porosity due to carbonation (confirmed by the MIP
results). After carbonation, the water absorption of the
RCA decreasd by 32·8, 30·9, 31·1 and 25·8% for the 2·5/5,
1·25/2·5, 0·63/1·25 and 0/0·63 mm fractions, respectively.
 Construction Materials Improving the properties of recycled
concrete aggregates by accelerated
carbonation
Zhao, Remond, Damidot, Courard and Michel

Therefore, carbon dioxide could be used to improve the prop- humidity on the carbonation of calcium hydroxide nanoparticles
erties of RCA. The influence of treated RCA on the properties and the formation of calcium carbonate polymorphs. Powder
Technology 205(1): 263–269.
of mortar and concrete will be studied in the next step (the
McNeil K and Kang THK (2013) Recycled concrete aggregates: a review.
properties of mortar and concrete should be improved as the International Journal of Concrete Structures and Materials 7(1):
quality of treated RCA is improved). The possibility of using 61–69.
carbon dioxide to improve the properties of RCA in industrial- Ngala V and Page C (1997) Effects of carbonation on pore structure
scale applications should also be considered exhaustively. and diffusional properties of hydrated cement pastes. Cement and
Concrete Research 27(7): 995–1007.
Poon CS, Kou SC and Lam L (2002) Use of recycled aggregates in
Acknowledgements molded concrete bricks and blocks. Construction and Building
The authors thank Lafarge for the supply of cement, Holcim Materials 16(5): 281–289.
Rao A, Jha KN and Misra S (2007) Use of aggregates from recycled
for the supply of natural aggregates and Colas for the supply of
construction and demolition waste in concrete. Resources,
RCA. They also thank the China Scholarship Council for finan- Conservation and Recycling 50(1): 71–81.
cial support. Finally, they thank the Government of Wallonia Sagoe-Crentsil KK, Brown T and Taylor AH (2001) Performance of
DGO6 for financial support through the project Beware concrete made with commercially produced coarse recycled
Academia CONRePaD (Design of concrete with recycled con- concrete aggregate. Cement and Concrete Research 31(5): 707–712.
Tam VWY, Wang K and Tam CM (2008) Assessing relationships among
crete aggregates by means of packing density method).
properties of demolished concrete, recycled aggregate and recycled
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caused by carbonation of cement mortar. Cement and Concrete
Research 31(6): 925–931. is available at www.icevirtuallibrary.com/page/authors,
López-Arce P, Gómez-Villalba LS, Martínez-Ramírez S, where you will also find detailed author guidelines.
Álvarez de Buergo M and Fort R (2011) Influence of relative

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