Construction and Building Materials 173 (2018) 754–762

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Construction and Building Materials

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

A procedure for characterizing the curing process of cold recycled

bitumen emulsion mixtures
Andrea Graziani a,⇑, Christian Iafelice b, Simone Raschia c, Daniel Perraton c, Alan Carter c
a
Department of Civil and Building Engineering, and Architecture, Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona, Italy
b
Università Politecnica delle Marche, Via Brecce Bianche, 60131 Ancona, Italy
c
Département de génie de la construction, École de technologie supérieure (ÉTS), 1100, Notre-Dame Street West, Montréal, Canada

h i g h l i g h t s g r a p h i c a l a b s t r a c t

A quantitative approach for

Cold-Recycled Mixtures (CRM)
measuring curing of cold recycled
mixtures is proposed.

Water and voids content had a
limited impact on the evolution of
indirect tensile strength. Reclaimed Asphalt Water Cement Bitumen Emulsion

A good correlation was found
between indirect tensile strength and
water loss. Curing

The water evaporation process was
virtually completed after 28 days.
Compaction Water loss & ITS

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

Article history: Due to the presence of water, emulsion and cement, cold recycled mixtures (CRM) are evolutive materials
Received 27 December 2017 and thus require a certain curing time to develop their long-term properties. The present study describes
Received in revised form 30 March 2018 a laboratory approach for characterizing the properties of CRM, focusing on their evolutive behaviour.
Accepted 9 April 2018
The experimental activities were carried out in parallel at the École de technologie supérieure (ÉTS) in
Available online 24 April 2018
Montréal, Canada and at the Università Politecnica delle Marche in Ancona (UNIVPM), Italy. The evolution
of water loss by evaporation and indirect tensile strength (ITS) was measured and analyzed using the
Keywords:
Michalis-Menten model, in order to achieve a quantitative characterization of the curing process. The
Bitumen emulsion
Bituminous pavements
results showed that different dosages of water resulted in different rates of water loss by evaporation,
Cement but did not penalize the development of ITS. Moreover, for both CRM, a good correlation was found
Cold recycling between water loss and ITS. Finally, the data showed that after 28 days of curing in the selected labora-
Curing tory conditions, the evaporation process was virtually completed.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction
The term cold recycling is associated to a broad series of cost-
effective and sustainable technologies for the rehabilitation of
bituminous pavements that are based on the use of reclaimed
asphalt (RA) as main aggregate source and bitumen emulsion or
foamed bitumen as main binders [1–3]. Ordinary Portland cement,
⇑ Corresponding author.
E-mail address: a.graziani@univpm.it (A. Graziani).
or other mineral additions like hydrated lime or fly ash, are gener-
ally used as secondary binders or as active fillers, in order to
improve the mechanical properties of cold recycled mixtures
(CRM). In the short term, the secondary binders allow an earlier
opening to commercial traffic whereas in the long term they
improve stiffness and strength of CRM layers [4–7]. Finally, water
is an essential component of CRM, because during mixing it con-
tributes to the homogeneous distribution of bitumen droplets
within the mixture, and thus leads to a good coating of aggregates
after emulsion breaking and setting [8–10].

https://doi.org/10.1016/j.conbuildmat.2018.04.091
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762
Because of the broad variability of component materials, mix-
ture compositions and production techniques, the mechanical
properties of CRM may be extremely variable. At least three
mixture families can be identified: bitumen stabilized materials
(characterized by high stress-dependency and failure in shear)
[11], cement-bitumen treated materials (stiffness and strength
properties depend on the balance between bitumen and cement)
[12–15] and cold-mix asphalts (aggregate fully coated with
bitumen and high thermal sensitivity) [16,17].
Despite such variability, a common distinctive feature of CRM is
their evolutive behavior [18–22]. In fact, physical and mechanical
properties of CRM require a certain curing time to evolve from
the short-term ‘‘fresh” state, to the long-term ‘‘hardened” state.
During curing, the water content reduces until reaching equilib-
rium with the surrounding environment within the pavement
structure, whereas mechanical properties improve until attaining
ultimate performance. Since both bituminous and hydraulic bin-
ders are generally present, the curing process of CRM occurs as a
result of the interaction of different physical and chemical mecha-
nisms, like emulsion breaking and setting and cement hydration.
Field curing is influenced by many factors, such as layer thick-
ness, drainage condition, construction sequence, temperature and
humidity. Thus, defining a curing process for laboratory investiga-
tions aimed at simulating field curing is very difficult. However, it
is imperative to develop laboratory curing methods that allow to
quantify differences in CRM behavior. This is obtained by fixing
boundary conditions in terms of temperature and humidity, and
carefully considering the effect of specimen-related properties like
shape, dimensions and voids.
Bearing in mind the previous aspects, the curing process of CRM
in the laboratory can be characterized in a quantitative way by
identifying two parameters [23]:

one parameter related to the CRM properties in the hardened
state, i.e. at the end of the curing process;

one parameter related to the initial rate of evolution of these
properties, i.e. the initial rate of the curing process.
A similar approach is used to identify the evolution of Portland
cement strength. For example, in the European Standard EN 197-1,
one parameter (the compressive strength of a normalized mortar
after 28 days of curing) is used to measure the strength in the hard-
ened state and one attribute (N or R) is used to indicate the rate of
strength increase at the beginning of the curing process.
1.1. Volumetric properties of CRM and their evolution
Volumetric properties of bituminous mixtures, either hot or
cold, have a significant influence on their mechanical performance
and durability. For cold mixtures, including CRM, it has to be con-
sidered that the volumetric composition changes during curing,
mainly due to water evaporation (Fig. 1). In addition, part of the
water that remains in the mixture actually changes its physical
state because is used for hydration of Portland cement. In general,
it is well known that the volume of the reaction products formed
during hydration is slightly lower than the cement and water
reacted [24].
The solid phase of CRM includes RA (aged bitumen is considered
part of the RA particles), virgin aggregate, filler and cement (or
other secondary binders). The bitumen droplets in the emulsion,
are actually ‘‘solid” and is assumed that they are not absorbed by
the aggregate which is wet condition at the mixing time. The total
water in the CRM is the sum of the water from the bitumen
emulsion and the water added during mixing. Part of the water
is absorbed by the aggregate, the rest is intergranular water
755
(also indicated as ‘‘free” water), and is available to enhance work-
ability, compaction and for cement hydration.
Curing causes a progressive increase of the volume occupied by
the voids and the solid phase (products of cement hydration),
whereas the volume of water progressively decreases, due to
evaporation and cement hydration. Evaporation also causes a mass
loss of the mixture that can be measured in the laboratory and in
the field in order to monitor the curing process [25]. Fig. 1 shows
typical changes of the volumetric composition of CRM over time.
The volumetric properties of CRM can be characterized by the
voids in the mixture (V m ) and the voids filled with liquids (VFL),
that are calculated as follows [9]:
V V;A þ V W;F V  ðV S þ V B;E Þ
Vm ¼ ¼ ð1Þ
V V
V B;E þ V W;F V B;E þ V W;F
VFL ¼ ¼ ð2Þ
V V;A þ V B;E þ V W;F V  VS
where V is the total volume of the specimen during compaction
(geometric volume based on the height of the specimen calculated
during compaction), V S is the bulk volume of solids (aggregates and
cement), V B;E is the volume of fresh bitumen (emulsion residue),
V W;F is the volume of free water and V V;A is the volume of intergran-
ular voids filled with air. It is highlighted that V S , V B;E and V W;F are
calculated using the initial mass of the materials and their density
(or specific gravity), whereas V V;A is calculated based on the total
volume of the specimen V (Eq. (2)). Therefore, the accuracy of
the calculations carried out using Eqs. (1) and (2) relies on the
hypothesis that material loss during compaction is negligible. This
hypothesis needs to be carefully checked after the compaction of
each specimen by comparing the mass of the material put in the
mold and the mass of the compacted specimens.
1.2. Analytical model for curing description
In order to describe the curing process of CRM in a quantitative
way, the development of physical and mechanical properties was
analyzed using the Michaelis-Menten (MM) model [26]. The MM
model was applied to describe the asymptotic increase of material
properties, for example water loss by evaporation (WL) and indi-
rect tensile strength (ITS), as a function of curing time t [23] as
follows:
yA  t
yðtÞ ¼ ð3Þ
hy þ t
where yðtÞ is the material property under investigation, yA is its
asymptotic value and hy is the curing time required for yðtÞ to reach
one half of the long-term value. The parameter hy can be used as a
measure of the initial curing rate: a lower value of hy indicates a fas-
ter increase of y in the first curing stage, i.e. up to yA =2. Both yA and
hy have a clear physical meaning, hence their values must to be
positive.
Eq. (3) may also be used to represent the relation between two
material properties, for example ITS (dependent variable) as a
function of WL (predictor). However, in this case, there is not an
asymptotic increase and thus the regression parameters yA and
hy do not have a clear physical meaning. In the initial curing stage,
if ITS increases faster than WL, i.e. if hITS < hWL , then Eq. (3)
describes a curve which is convex upward (concave curve) [27].
This indicates that cement hydration (which is not directly related
to water loss) has a marked effect on ITS increase rate. Vice versa, if
hWL < hITS , Eq. (3) describes a curve which is convex downward
(convex curve). This indicates that emulsion breaking (which is
directly related to water loss) controls the ITS increase rate. It
can also be observed that, in the limiting case of hITS ¼ hWL ,
756 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762

Fig. 1. Volumetric composition of CRM and evolution over time.

Eq. (3) degenerates into a straight line, with a slope equal to the In the first part of the study, a reference CRM composition was
ratio between the asymptotic values of ITS and WL. identified in terms of grading curve, minimum RA content, bitu-
men emulsion content and Portland cement content. Then, locally
available materials were selected and characterized using the rele-
2. Research significance
vant testing standards. ÉTS and UNIVPM adopted similar mixing
and compaction procedures, and performed preliminary tests in
A meaningful comparison between different CRM must address
order to select the water content of the CRM, according to volumet-
the evolution of their volumetric and mechanical properties
ric criteria.
throughout the curing process. For example, CRM having similar
In the second part of the study, two mixtures were produced:
strength after full curing, may achieve very different strength after
one at ÉTS (Mixture-CA) and one at UNIVPM (Mixture-IT). Each
a few hours or days, which will have an effect on traffic opening
laboratory prepared a series of testing specimens and recorded
time. On the other hand, CRM designed to reach high strength at
the water loss (WL) by evaporation and the indirect tensile
the beginning of the curing process, may achieve very different
strength (ITS), until 28 days, in fixed curing conditions. The evolu-
ultimate strength values, which will have an effect on the thickness
tion of these properties was analyzed using a simple analytical
of the pavement, or on its long-term performance.
model, which allows the identification of a parameter representing
The objective of this paper is to describe a procedure for charac-
their long-term value and a parameter representing their rate of
terizing the curing process of CRM, in order to compare different
evolution.
mixtures based on their evolutive behavior. Specifically, the proce-
dure is applied considering two CRM with similar composition, but
produced in different countries and with different materials. 3. Materials and methods
The experimental work was carried out in parallel at the École
de technologie supérieure (ÉTS) in Montréal, Canada and at the 3.1. Materials
Università Politecnica delle Marche (UNIVPM) in Ancona, Italy. A
further objective of this study was to compare the properties of The main geometrical and physical properties of the two RA
CRM prepared following North American and European practices sources used in this study are summarized in Table 1 and their
and standards. grading curves are reported in Fig. 2.

Table 1
Main properties of RA sources.

Property Standard Value

RA – IT
Binder content (by mass of aggregate) EN 12697-1 5.66%
Nominal maximum particle dimension EN 13108-8 16 mm
Apparent density: qa (particles passing the 4 mm sieve) EN 1097-6 2 492 kg/m3
Apparent density: qa (particles retained on the 4 mm sieve) EN 1097-6 2 609 kg/m3
Water absorption (particles passing the 4 mm sieve) EN 1097-6 0.3%
Water absorption (particles retained on the 4 mm sieve) EN 1097-6 0.6%
Fragmentation @5 °C (fraction 5/10) –%passing 1.6 mm sieve EN 13286-50 7.7%
Fragmentation @20 °C (fraction 5/10) –%passing 1.6 mm sieve EN 13286-50 7.6%
RA – CA
Binder content (by mass of aggregate) LC 26-006 6.10%
Nominal maximum particle dimension LC 21-010 10 mm
Maximum Specific Gravity: Gmm LC 26-045 2.577
Water absorption (particles passing the 2.5 mm sieve) LC 21-065 2.3%
Water absorption (fraction 2.5/5 mm) LC 21-066 1.9%
Water absorption (particles retained on 5 mm sieve) LC 21-067 1.6%
Fragmentation @5 °C (fraction 5/10) –%passing 1.6 mm sieve EN 13286-50 9.6%
Fragmentation @20 °C (fraction 5/10) –%passing 1.6 mm sieve EN 13286-50 8.6%
 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762 757

require a well-graded mixture, closer to the maximum density

curve [31]. In this study, for both Mixture-IT and Mixture-CA, the
design gradation (by volume) was chosen according to the Fuller-
Thompson equation, with exponent 0.45 (Fig. 2). The maximum
aggregate size of Mixture-CA is 10 mm and 16 mm for Mixture-
IT. For Mixture-IT, the target blend was composed of RA (75.8%),
a 0/4 limestone sand (15.8%) and a limestone filler (6.9%), whereas
for Mixture-CA, the target blend was composed of RA (91.0%) and
limestone filler (7.5%). It is highlighted that the CRM gradation
was designed including the volume of Portland cement whose
dosage was fixed at 1.5% by mass of aggregate, for both CRM. The
fresh bitumen content was also fixed at 2% by mass of aggregate,
corresponding to an emulsion dosage of 3.3%, for both CRM.

3.2. Mixing and compaction

Fig. 2. Grading curves of RA sources and design aggregate blends. Laboratory mixing of the CRM was carried out in two phases. In
the first phase, dry aggregates (RA, sand and filler) were combined
and an amount of water corresponding to the absorption of RA and
In defining the CRM composition, RA is considered as a ‘‘black
sand was added. The moist blend was enclosed in a sealed bag and
rock”, i.e. the aged bitumen is considered part of the aggregate par-
maintained at room temperature for at least 12 h prior to mix in
ticles. This means that, even though the aged bitumen changes the
order to ensure a homogeneous moisture condition and to allow
properties of the original aggregate particles, it is not considered as
water absorption by the aggregate particles. In the second phase,
‘‘binding phase”. Indeed, since the production of CRM is carried out
binders and water were added in the following order: Portland
at ambient temperature, blending between the aged binder in RA
cement, water (half of the required amount), bitumen emulsion
and the fresh binder in the bitumen emulsion is questionable.
and finally the second half of the required water amount. After
At UNIVPM, the RA ‘‘apparent density” qa was measured using
each addition, the blend was thoroughly mixed until obtaining a
the testing standard for aggregates (EN 1097-6) [28], whereas at
uniform aspect (Fig. 3a-b). The whole mixing process typically
ÉTS the RA ‘‘specific gravity” was measured according to the stan-
required six to eight minutes, starting from cement addition.
dard adopted for measuring the maximum specific gravity of bitu-
Specimen compaction was carried out immediately after mix-
minous paving mixtures Gmm (ASTM D2041) [29]. It is underlined
ing, using a gyratory compactor. The following compaction proto-
that both qa and Gmm are calculated from the ratio of the dry mass
col was adopted: undrained mold with D = 150 mm, constant
and the particle volume, including the impermeable voids but not
pressure of 600 kPa, gyration rate of 30 rpm and external angle
the permeable voids. The fragmentation test was performed on RA
of inclination of 1.25°. After compaction, the cylindrical specimens
sources, according the procedure described in [30]. This test, which
were immediately extracted from the mold and weighted in order
basically consists in measuring the amount of fine particle (passing
to check any material loss (Fig. 3c-d). The final (average) height at
the 1.6 mm sieve) produced during Proctor compaction, was
the end of compaction was 72.0 and 74.4 mm for specimens pro-
recently introduced as a quick test to check the dimensional stabil-
duced at ÉTS and UNIVPM, respectively.
ity and the overall quality of RA.
In this study, preliminary compaction tests were carried out in
Cationic slow-setting bitumen emulsions were used at both ÉTS
order to check the compactability of the mixtures and identify a
and UNIVPM, their main properties (as declared by the manufac-
target water content for the testing specimens, based on their vol-
turers) are summarized in Table 2. The cement used at ÉTS was a
umetric properties. The basic steps of the procedure were as
type GU (CSA A3000) with compressive strength at 28 days of
follows:
43.9 MPa (ASTM C 109), whereas the cement used at UNIVPM
was a CEM II/A-LL (EN 197-1) with strength class 42.5R. Both
1. compact specimens at different water contents and monitor the
cements had a Blaine fineness of 410 m2/kg and may be considered
effect on Vm (water enhances compaction resulting in a
to be the same type.
decrease of Vm );
In the region of Quebec, requirements for the gradation of the
2. check the values of VFL (the values of Vm make sense only if VFL
aggregate blend provided by the Ministère du Transport du
< 100%);
Québec, are very wide. On the other hand, Italian specifications
3. check for any loss of water and fines (including cement and
bitumen droplets) at the end of compaction (loss of material
may start at VFL values grater than 85%).
Table 2
Main properties of bitumen emulsions.
The preliminary compaction tests revealed that the mixture
Property Standard Value produced at ÉTS had lower V m with respect to the mixture pro-
Emulsion – IT duced at UNIVPM, when compacted at the same number of gyra-
Designation EN 13808 C60B10 tions and at the same, or even at lower, water content. Based on
Nominal Binder Content EN 1428 60.0% these results, the free water content of Mixture-CA was fixed at
Viscosity at 40 °C (efflux time) EN 12486-1 40 s 2%, by mass of solids (corresponding to a total water content of
Mixing stability with cement EN 12848 <2%
Penetration (recovered binder) EN 1426 70 mm/10
2.9%), whereas the free water content of Mixture-IT was fixed at
4% by mass of solids (corresponding to a total water content of
Emulsion – CA
Type ASTM D2397 CSS-1
4.9%). In order to illustrate the compactability of the mixtures,
Distillation residue at 260 °C ASTM D6997 62.8% Fig. 4 reports the upper and lower bounds of the compaction
Viscosity Saybolt-Furol at 25 °C ASTM D7496 28.1 s curves of all the tested specimens. As it can be observed, 180 gyra-
Oversized Particles ASTM D6933 < 2% tions were necessary to decrease the V m of Mixture-IT to an aver-
Penetration (recovered binder) ASTM D5 170 mm/10
age value of 9.0%, whereas V m of Mixture-CA reached an average
758 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762
Fig. 3. Mixing and compaction phases: a) adding of bitumen emulsion (ÉTS); b) hand-mixing (ÉTS); c) compaction mold (UNIVPM); specimen extraction (UNIVPM).
Fig. 4. Upper and lower bounds of compaction curves for the tested CRM specimens: a) Vm vs. Gyrations; b) VFL vs. Gyrations.
value of 5.5% after less than 90 gyrations. Those V m were selected
based on an average VFL of 90%.
3.3. Testing
A series of 15 testing specimens was produced, cured and tested
both at ÉTS (Mixture-CA) and UNIVPM (Mixture-IT). According to
Canadian and Italian practices, the ÉTS specimens were cured at
35 °C and 65 ± 5% relative humidity, whereas the UNIVPM speci-
mens were cured at 40 °C and 65 ± 5% relative humidity. Water
evaporation was allowed while curing in both cases. The indirect
tensile strength (ITS) of the cured specimens was measured after
1, 3, 7, 14 and 28 days (three replicate specimens at each age).
ITS tests were carried out at 20 °C, therefore specimens cured at
both 35 °C and 40 °C were conditioned for 4 h at 20 °C before test-
ing. The load was applied with a constant rate of displacement of
50 ± 2 mm/min (Fig. 5). Before mechanical testing the WL was
assessed by weighting each specimen.
4. Results and discussion
4.1. Development of material properties
The development in time of WL and ITS is shown in Figs. 6 and
7. The WL values measured for Mixture-CA range from 1.3% (1 day)
to 2.6% (28 days), whereas the values measured for Mixture-IT
range from 2.6% (1 day) to 4.4% (28 days). The difference between
these ranges can be related to the difference between the initial
water content of the CRM (2.9% and 4.9%). On the other hand,
the ranges of variability of ITS, from 368 kPa to 754 kPa for
Mixture-CA and from 345 kPa to 699 kPa for Mixture-IT, are very
similar.
It is important to note that, even if Mixture-CA is characterized
by lower dosage of water and lower voids (V m = 5.5%), with respect
to Mixture-IT (V m = 9.0%), the long-term ITS value of the two mix-
tures is very similar (709 and 697 kPa). This is an unexpected find-
ing and suggests that the long term mechanical performance of
CRM is mostly related to other factors like the grading curve, the
quality of RA aggregate and the dosages of residual bitumen and
cement.
In Figs. 6 and 7, the continuous lines superposed to the experi-
mental data represent the fitted MM model. The values of the
regression parameters (yA and hy ) and their standard errors, were
estimated using nonlinear least-squares minimization [32] and
are reported in Table 3. A visual check of the regression quality
shows that the fitted models underestimate the values of WL and
ITS measured after 28 days of curing. This is confirmed by the esti-
mated asymptotic values of both WL and ITS, which are lower with
respect to the values actually measured at 28 days. However, the
overall precision of the models, as measured by the residual stan-
dard errors reported in Table 3, appears to be quite good for both
 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762 759

Mixture-CA

Mixture-IT

a) b) c)
Fig. 5. ITS measurement: a) testing at ÉTS; b) testing at UNIVPM; c) cut section of tested specimens.

Fig. 6. Development of WL with superposed fitted MM model.

Fig. 7. Development of ITS, with superposed fitted MM model.

760 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762
Table 3
Fitted parameters of the MM model for time development of WL and ITS.
Mixture yA
Estimate Std. Error
WL vs. time
Mixture-CA 2.37% 0.10%
Mixture-IT 4.16% 0.12%
ITS vs. time
Mixture-CA 709 kPa 26 kPa
Mixture-IT 697 kPa 30 kPa
Fig. 8. Normal QQ plot: a) MM model for WL; b) MM model for ITS.
CRM. The normal quantile-quantile (QQ) plots for the residuals of
WL and ITS are reported in Fig. 8. Although some issues are present
for ITS data measured at UNIVPM (Mixture-IT), the data points plot
reasonably well along the equality line, confirming that for both
properties the errors of the MM model may be considered nor-
mally distributed.
Analyzing the values of hy it is observed that in the first curing
stage (i.e. up to yA =2) Mixture-IT showed a faster water loss with
respect to Mixture-CA (0.81 days versus 1.20 days), but a slower
increase in ITS (1.46 days versus 1.21 days). This can be related
to the fact that, in this initial phase, Mixture-IT is characterized
by higher water content and higher voids with respect to
Mixture-CA. These factors contribute to enhance water loss by
evaporation and delay the development of strength. However, as
curing proceeds, the ITS of Mixture-IT gets closer to the ITS of
Mixture-CA, as confirmed by the asymptotic values (697 kPa ver-
sus 709 kPa).
Previous studies highlighted that differences in curing temper-
ature as high as 15 °C, had an impact mainly on the initial curing
rate (higher temperatures led to lower hy values) [23]. The results
of the present study show that, at least for ITS, the different curing
temperature (35 °C at ÉTS, 40 °C at UNIVPM) had a limited effect. If
present, this effect was concealed by the effect of other factors,
such as, for example, the different initial water content between
the two CRM.
4.2. Relationship between water loss and ITS
The evolution of WL and ITS discussed in the previous section is
closely related to the specimen geometry and boundary conditions
(e.g. curing temperature and RH). The value of the initial curing
hy Residual
Estimate Std. Error Std. Error
1.20 days 0.27 days 0.22%
0.81 days 0.14 days 0.28%
1.21 days 0.23 days 55 kPa
1.45 days 0.30 days 60 kPa
rate hy may be used for comparing different mixtures in the labo-
ratory, but its extension to a pavement-scale curing processes is
not straightforward. Indeed, when the MM model has been applied
to analyze field curing of CRM, hy values as high as 6 days were
estimated [25]. However, the experimental data also allow estab-
lishing a direct relationship between WL and ITS. The data were fit-
ted using Eq. (3), the regression lines are superposed to the
experimental data in Fig. 9a and the regression parameters are
summarized in Table 4. It can be observed that for Mixture-CA
the regression is almost linear, suggesting that during curing ITS
increases at the same rate of WL (in fact the models WL(t) and
ITS(t) are characterized by almost equal hy values: 1.20 and 1.21
days). For Mixture-IT Eq. (3) produces a convex curve because in
the initial curing stage WL is faster than ITS increase.
The next step is to analyze the ITS increase considering the
residual water content of the mixtures instead of the water loss.
The residual water has been calculated simply as the difference
between the initial water content and WL. The relationship is
depicted in Fig. 9b, where the lines superposed to the experimental
data represent the same models described in Fig. 9a and in Table 4.
Fig. 9b confirms that, in the initial curing stage, the higher water
content of Mixture-IT did not penalize the ITS of the mixture. As
curing proceeds, the residual water content of the two mixtures
becomes almost zero and their ITS approaches the maximum
value.
As highlighted in Section 2.3, a fraction of the water in the CRM
is used for hydration of Portland cement. According to Powers’ the-
ory, per 100 g of cement reacted, 23 g of water are chemically
bounded and hence are not available for evaporation [24]. For
the CRM considered in the present research, assuming a degree
of hydration of 0.9 after 28 days [33], the chemically bounded
 A. Graziani et al. / Construction and Building Materials 173 (2018) 754–762
Fig. 9. Relationship between residual water and ITS, with fitted MM model: a) ITS vs. WL; b) ITS vs. residual water (arrows show the effect of curing).
Table 4
Fitted Parameters of the MM Model for ITS vs. WL.
Mixture yA
Estimate Std. Error
Mixture-CA 11.10 14.41
Mixture-IT 1.69 0.67
water content is about 0.45%. Thus, Fig. 9b also indicates that after
28 days the evaporation process is nearly completed for both mix-
tures, despite the fact that their initial water content and the cur-
ing temperature were different.
5. Conclusions
In the present study, a procedure for characterizing the curing
process of CRM was applied considering two CRM produced at
the Università Politecnica delle Marche in Ancona (Italy) and at
the École de technologie supérieure in Montréal (Canada). In par-
ticular, the Michaelis-Menten model was applied to get a quantita-
tive comparison between the mixtures, in terms of ITS and water
loss. From the comparison of the two mixtures it was observed
that, because of the higher dosage of water, Mixture-IT was charac-
terized by a faster water loss in the initial curing stage, with
respect to Mixture-CA. On the other hand, Mixture-CA was charac-
terized by a faster increase of ITS in the initial curing stage, with
respect to Mixture-IT. However, in the long-term, the ITS of the
mixtures was very similar, suggesting that for the studied mixtures
water dosage and air voids content have a limited impact on
mechanical performance. For both CRM, a good correlation was
found between ITS and water loss; this correlation may be
extended to analyze field curing conditions. When considering
the amount of water chemically and physically bound by cement,
the experimental data showed that for both CRM the evaporation
process was virtually completed after 28 days.
Conflict of interest
The Authors declare no conflict of interest
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