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Effect of Cement C3A Content on Properties of Cementitious Systems

Containing High-Range Water-Reducing Admixture

Article  in  Journal of Materials in Civil Engineering · April 2017

DOI: 10.1061/(ASCE)MT.1943-5533.0001925

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 Effect of Cement C3A Content on Properties of
Cementitious Systems Containing High-Range
Water-Reducing Admixture
Ali Mardani-Aghabaglou, Ph.D. 1; Burak Felekoğlu, Ph.D. 2; and Kambiz Ramyar, Ph.D. 3

Abstract: The effect of cement tricalcium aluminate (C3 A) content on the properties of cement paste, mortar, and concrete mixtures
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containing high-range water-reducing (HRWR) admixture was investigated. Three commercial Type I cements prepared with the same
raw material and same gypsum rock interground with clinker, but with different C3 A contents (by changing mixture proportions), were
used. The fresh state, rheological properties, and compressive strength of the mixtures were studied. Moreover, X-ray diffraction (XRD)
patterns of 6-h-age paste mixtures from each cement were obtained. By reducing the C3 A content of the cements, the fresh state, rheological,
and consistency retention properties of the mixtures improved; however, the strength of the mixtures at early ages decreased. The difference
between strength of the mixtures closed at later ages. The XRD analysis of the pastes revealed the formation of more ettringite
in the paste prepared from high C3 A content cement. DOI: 10.1061/(ASCE)MT.1943-5533.0001925. © 2017 American Society of Civil
Engineers.
Author keywords: Cement C3 A content; Fresh properties; Rheological parameters; X-ray diffraction analysis.

Introduction Ramachandran 1995). The cement tricalcium aluminate (C3 A) con-

To improve the properties of fresh and hardened concrete, the use of
chemical admixtures in the concrete or mortar mixtures is inevi-
table. Plasticizers and superplasticizers are the most widely used
types of chemical admixtures in the concrete industry. The chemi-
cal admixtures used in concrete not only may cause expected pos-
itive effects, but sometimes unexpected negative effects as well
(Kantro 1980; Schatzmann et al. 2003, 2004; Koehler and Fowler
2004; Perenchio et al. 1979; Tagnit-Hamou and Aïtcin 1993).
Rixom and Mailvaganam (1986) and Akman (1996) reported that
for a given workability, the use of plasticizer and superplasticizer
admixtures in the concrete may reduce water demand by as much as
6.5 and 12–16%, and an increase in compressive strength may be
more than 10 and 15%, respectively. The cement–admixture incom-
patibility may affect the fresh state and hardened properties of the
concrete. The negative effects arising from the use of plasticizers
are set retarding, slump loss, excessive air entrainment, and increas-
ing risk of shrinkage. In addition, superplasticizers may cause loss
of workability and may increase the risk of segregation and drying-
shrinkage if used unconsciously (Bedard and Mailvaganam 2003;
Dodson and Hayden 1989; Bonen and Sakar 1995; Erdoğdu
2000; Jiang et al. 1999). Some of the factors responsible for these
negative effects may be from the cement and others from the
water-reducing admixture (Bedard and Mailvaganam 2003;
1
Assistant Professor, Dept. of Civil Engineering, Univ. of Uludağ,
Nilüfer-Bursa 16059, Turkey (corresponding author). E-mail: ali
.mardani16@gmail.com
2
Associate Professor, Dept. of Civil Engineering, Univ. of Dokuz Eylul,
Buca-Izmir 35220, Turkey.
3
Professor, Dept. of Civil Engineering, Univ. of Ege, Bornova-Izmir
35040, Turkey.
Note. This manuscript was submitted on August 9, 2016; approved on
December 29, 2016; published online on April 3, 2017. Discussion period
open until September 3, 2017; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
tent is one of the most important factors affecting the cement-water
reducing admixture compatibility. Tricalcium aluminate is the most
highly reactive phase in clinker and the one with the greatest affin-
ity for superplasticizer admixtures. The C3 A and sulfur trioxide
(SO3 ) content of the cement, and the type and amount of the ad-
mixture, largely influence the paste, mortar, and concrete rheologi-
cal behavior (Alonso and Puertas 2015).
Modification of the formation rate and surface area of ettringite
by polycarboxylate ether–based superplasticizer admixtures during
early C3 A-calcium sulfate (CaSO4 ) hydration was investigated by
Dalasa et al. (2015). For this aim, two polycarboxylate ether–based
superplasticizer admixtures differing in their grafting degree were
used. In this study, the amount and specific surface area of the
ettringite formed upon the C3 A-CaSO4 hydration in the presence
or absence of the superplasticizer admixture were measured. Test
results demonstrated that the primary effect of superplasticizer ad-
mixtures was to increase ettringite-specific area strongly for a var-
iable period. The effect that was reduced by the delayed addition of
the admixture was attributed to the superplasticizer admixtures
charge and its dosage.
The adsorption of polycarboxylate and naphthalene ether–based
superplasticizer admixtures on cubic and orthorhombic C3 A was
investigated by Alonso and Puertas (2015). It was concluded that
the admixture structure and sulfate content of the system were the
factors with the greatest impact on the adsorption of admixture on
the cubic C3 A. Orthorhombic C3 A, reacting more intensely in the
presence of sulfate, showed less affinity for the admixtures. The
presence of superplasticizer admixtures had no effect on the peak
heat flow time in orthorhombic-C3 A hydration.
The amount of C3 A and alkali-sulfate added in the sequence
of the superplasticizer on the formation of the organo-mineral
phase were investigated by Habbaba et al. (2014). For this rea-
son, six commercial cements with different C3 A content—four
different polycarboxylate ether–based and one naphthalene ether–
based superplasticizer admixtures—were used. The admixtures
were added to the paste mixtures either with early or with delayed

© ASCE 04017066-1 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2017, 29(8): 04017066

 addition. It was found that the alkali-sulfates and C3 A content of Table 1. Chemical Composition and Physical Properties of Cements
cement play the key roles in terms of fresh properties of cement Item C5.85 C2.77 C1.90
paste mixtures. For cements exhibiting a low alkali-sulfate=C3 A
Chemical composition
molar ratio (0.04–1.29), huge differences in paste flow at early and
SiO2 19.85 18.77 18.95
delayed addition were observed, presumably because of chemi- Al2 O3 4.41 3.67 3.66
sorption (intercalation) of superplasticizer admixture into C3 A hy- Fe2 O3 4.14 5.05 4.95
drates (Giraudeau 2009). Whereas at high alkali-sulfate=C3 A molar CaO 61.05 64.27 63.91
ratios (∼2), ettringite predominantly was formed and superplasti- MgO 1.68 1.38 1.52
cizer admixture intercalation was impossible. Consequently, simi- Na2 O 0.27 0.20 0.24
lar flow values were attained at early and delayed addition. K2 O 0.50 0.62 0.41
There are many literature studies about the effect of cement C3 A SO3 3.16 3.17 2.81
content on rheological properties of the cementitious systems con- Cl− — 0.006 0.006
taining high-range water-reducing admixture (HRWR). Moreover, free CaO 1.37 1.42 1.97
LOI 3.3 1.40 1.64
there are many literature studies about the cement-water reducing
Total 99.73 99.96 100.06
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admixture compatibility (Grabiec and Piasta 2004; Kadri et al. 2009;

He et al. 2012; Wang et al. 2012; de Reese et al. 2013; Mardani- Physical properties
Aghabaglou 2016; Mardani-Aghabaglou et al. 2016). However, Specific gravity 3.14 3.16 3.16
there is no exact conclusion about this subject because the number Setting time (h)
of the affecting factors is quite excessive. In this study, the effect of Initial 02:50 02:50 03:30
Final 05:10 05:15 05:25
cement C3 A content on the rheological and fresh properties and
Vicat water (%) 30.2 30.8 30.4
compressive strength of cementitious systems containing HRWR
admixture were investigated. For this purpose, three commercial Fineness
CEM I 42.5 cements prepared from the same raw materials in the Blaine specific surface (cm2 =g) 4,260 3,820 3,760
same plant, but having different C3 A content, were used. This is not Residual on 0.090 mm sieve (%) 0.2 0 0
the case in previous studies conducted by the other researchers in Residual on 0.045 mm sieve (%) 1.4 1.7 2
Residual on 0.032 mm sieve (%) 6.6 7.2 7.9
which the difference between the cements used was not limited to
the C3 A content of the cements, but to their other properties arising
from their different raw materials, gypsum type, or production tech- Table 2. Chemical Composition of Clinkers and Gypsum Rock
nology. Paste, mortar, and concrete mixtures with different water–
cement (W/C) ratios were prepared. Fresh properties of the paste Clinker Gypsum rock
that added to
mixtures, such as Marsh-funnel flow time, miniflow, dynamic and
Item (%) C5.85 C2.77 C1.90 the clinkera
static yield stress, and final viscosity were investigated. In addition,
X-ray diffraction (XRD) analysis was performed on 6-hour (h)-age SiO2 21.13 21.24 21.14 3.48
paste mixtures to observe the level of ettringite formed in the paste. Al2 O3 5.07 4.4 4.13 0.58
Fe2 O3 4.48 5.25 5.35 0.4
Admixture requirement; flow; time-dependent flow loss; V-funnel
CaO 65.83 65.67 65.7 32.09
flow time; time-dependent loss of V-funnel flow time; rheological MgO 1.36 1.4 1.38 1.36
properties; and 1, 3, 7, and 28-day compressive strength were in- Na2 O 0.30 0.32 0.32 0.47
vestigated in mortar mixtures. In the concrete mixtures, bulk den- K2 O 0.52 0.45 0.45 0.14
sity; air content; slump; flow; time-dependent flow; slump loss; and SO3 0.48 0.45 0.51 38.51
1, 3, 7, and 28-day compressive strength tests were performed. Cl− 0.008 0.009 0.015 —
Free CaO 1.02 1.18 1.39 22.85
C3 S 62.83 64.03 65.73 —
Materials, Mix Preparation, and Test Procedures C2 S 13.20 12.63 11.05 —
C3 A 5.85 2.77 1.90 —
Materials C4 AF 13.63 15.98 16.27 —
a
The same gypsum rock was used in all of the cements.
Three CEM I 42.5 type cements with different C3 A contents con-
forming to the EN 197-1 (CEN 2010a) standard were used as binders
in this study. The raw materials of the cements and the gypsum rock absorption capacity of the aggregates conforming to the EN 1097-6
added during grinding were the same. The proportions of raw ma- (CEN 2007) standard are shown in Table 3. To provide the desired
terials varied to prepare clinkers with different C3 A contents. De- workability, polycarboxylate ether–based HRWR admixture was
pending on their C3 A contents (5.85, 2.77, and 1.90%), the cements used. Properties of the admixture, given by its producer, are shown
were designated as C5.85 , C2.77 , and C1.90 , respectively. Chemical in Table 4.
composition of the cements, clinker, gypsum rock, and mechanical
and physical properties of the cements are shown in Tables 1 and 2.
Experimental study was conducted in three stages. In the first Mixture Preparation
stage, paste mixtures were prepared and the effect of cement C3 A The preparation of paste, mortar, and concrete mixtures are given
content on fresh state properties of the mixtures was investigated. elsewhere in detail (Mardani-Aghabaglou et al. 2016), however,
In the second stage, mortar mixtures were prepared with standard for the sake of convenience, these are repeated briefly in this
sand. The third stage included the tests of concrete mixtures. manuscript.
Crushed limestone aggregate in four different size fractions (0–3,
0–5, 5–15, and 15–25 mm), with 25 mm maximum grain size, was
Preparation of Cement Paste Mixture
used. The proportions of these size fractions were adjusted to ob-
tain a combined aggregate having a gradation conforming to EN Regarding previous studies for the Marsh-funnel and minislump
206 (CEN 2013), as shown in Fig. 1. The specific gravity and water tests, the W/C ratio of the paste mixtures was chosen as 0.35.

© ASCE 04017066-2 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2017, 29(8): 04017066

 Minimum limit Maximum
Maksimumlimit
limit Mixture Table 5. Scanning for Determination of Rheological Properties of Mortar
Mixtures
100
W/C ratio
90
0.40 0.50 0.60 0.80
80 Admixture dosage
(wt.% of cement) C1.90 =C2.77 =C5.85
70
Passing (%)

0 x/x/x x/x/x OK/OK/OK S/S/S

60
0.1 x/x/x x/x/x OK/OK/OK S/S/S
50 0.2 x/x/x OK/OK/OK OK/S/S S/S/S
40 0.3 x/x/x OK/OK/OK S/S/S S/S/S
0.4 x/x/x OK/S/S S/S/S S/S/S
30
0.5 x/x/x S/S/S S/S/S S/S/S
20 0.6 x/x/x S/S/S S/S/S S/S/S
10 0.7 x/x/x S/S/S S/S/S S/S/S
0.8 x/OK/OK S/S/S S/S/S S/S/S
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0
0.125 0.25 0.5 1 2 4 8 16 32 Note: OK = mixture suitable for measurement; S = liable to segregation;
Sieve size (mm) X = over-stiff.

Fig. 1. Gradation curve of combined aggregate and EN 206 (CEN

2013) standard limits Table 6. Corrected Mix Proportions of Concrete Mixtures (kg=m3 ) and
Some Fresh Properties
Mix C5.85 C2.77 C1.90
Table 3. Physical Properties of Aggregates Used in Concrete Mixtures Cement 392 393 393
Water 176 177 177
Property 0–3 mm 0–5 mm 5–15 mm 15–25 mm
Super plasticizer admixture 4.3 4.1 3.7
Apparent specific gravity 2.71 2.74 2.68 2.69 Aggregate (SSD) (mm)
SSD bulk specific gravity 2.66 2.70 2.66 2.67 0–3 747 750 751
Water absorption capacity (%) 1.15 0.75 0.45 0.45 0–5 379 381 381
Loose unit weight (kg=m3 ) 1,780 1,730 1,515 1,490 5–15 373 375 376
15-25 375 376 377
Unit weight (kg=m3 )
Table 4. Properties of Polycarboxylate Ether–Based HRWR Admixture Theoretical 2,424.7 2,427.5 2,427.5
Property Value Measured-fresh 2,441 2,420 2,420
Measured-hardened (SSD) 2,519 2,452 2,455
Alkali content (%) (Na2 O) <5 ΣPaste 572 574 574
Density (g=cm3 ) 1.098 ΣMortar 1,698 1,705 1,706
Solids content (%) 35.73
Chloride content (%) 0.012 Fresh properties
pH, 25°C 5.97 Air content (%) 1.8 1.9 1.6
Operating range (%)a 0.6–2.0 Slump value (mm) 220 230 230
a Flow value (mm) 480 490 490
By weight of cement.

For each cement type, in addition to the control mixture containing
no chemical admixture, six different mixtures containing HRWR
admixture, ranging from 0.5% to 1.75 wt.% of cement, were pre-
pared. However, to investigate the rheological characteristics for
the rheometer capacity and segregation tendency of the mixtures,
two different W/C ratios (0.35 and 0.32) and three different admix-
ture dosages (0, 0.1, and 0.2 wt.% of cement) were adapted to ob-
tain six different mortar mixtures for each cement. When the W/C
ratio of the mixture was more than 0.35, the admixture requirement
was negligible. Conversely, when the W/C ratio was less than 0.32,
the mixtures were too stiff to be tested by the available rheometer.
Preparation of Mortar Mixtures
Mortar mixtures were prepared in compliance with ASTM C109
(ASTM 2013b). Water-cement ratio, sand/cement (S/C) ratio, and
flow value were kept constant at 0.485, 2.75, and 270
10 mm,
respectively, in all of the mixtures. The desired flow value was ob-
tained by using HRWR admixture. For the rheometer capacity and
properties of the prepared mixtures (very stiff or liable to segrega-
tion), a preliminary study was performed to select the proper W/C
ratios and admixture dosages in the mixtures. The results shown in
Table 5 revealed the appropriate W/C ratios as 0.5 and 0.6. In
addition, the proper admixture dosages for the mixtures having
a 0.5 W/C ratio were determined as 0.2 and 0.3 wt.% of the cement.
The corresponding values for the mixtures having 0.6 W/C ratio
were 0 and 0.1%. In this way, the rheological properties were de-
termined in mixtures with 0.5 and 0.6 W/C ratios and different
admixture dosages.
Preparation of Concrete Mixtures
Three concrete mixtures having a constant W/C ratio (0.45) and
a constant slump (225
5 mm) were prepared in accordance
with ACI 211 (ACI 1998) recommendations. The corrected mix
proportions and some properties of the fresh mixtures are given in
Table 6.
Test Procedures
Cement Paste Test Methods
The Marsh-funnel flow time and minislump values of the paste
mixtures were obtained by the methods proposed by Aïtcin (2004)
and Kantro (1980), respectively.

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 A rheometer with a ball measuring system (BMS) was used to
obtain the rheological properties of the paste mixtures (Schatzmann
et al. 2004, 2003; Felekoğlu 2014). The highest shear rate in this
rheometer was 35 s−1 . This value is equivalent to the movement of
an 8-mm diameter steel ball at a speed of 60 rpm. Moreover, the
maximum moment value to be measured was 125 Millinewtonmetre
(mNm). For this reason, the maximum shear stress measurable by
the rheometer was 2,850 Pa. The shear rate history applied in
the study and its four periods are shown in Fig. 2. Each period
is described briefly below.
1. The ball was lowered to the measuring point in the undisturbed
mixture and moved at a constant shear rate of 0.5 s−1 . The mo-
ment was measured at 2 s intervals for a period of 60 s. The peak
point of the shear stress-time diagram was accepted as static
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yield stress of the mixture.
2. The second period was applied to remove the shear history in the
mixture arising from its mixing. For this purpose, the ball was
rotated with a 5 s−1 constant shear rate for 30 s.
3. In this period, the shear rate was increased from 0 to 30 s−1
at 150 s.
4. In this period, the shear rate was decreased from 30 to 0 s−1 at
150 s. The moment was measured at 5 s time intervals.
Finally, the rotational speed (Ω) and moment (T) obtained dur-
•
ing the experiment were turned into shear rate (γ ) and shear stress
(τ ), respectively, by the help of empirical coefficients defined in
the RheoPlus software program (Chen et al. 2016). Details of
the determination methodology of empirical coefficients can be
found in Schatzmann et al. (2004).
The dynamic yield stress was obtained by plotting the flow curve
of the mixture with the data of Period 4 by using the Herschel-Bulkley
model (Mardani-Aghabaglou et al. 2016). The intersection of the flow
curve with y-axis was taken as a dynamic yield stress. The viscosity
value measured in the Herschel-Bulkley model is not a constant value,
but, in most cases, decreases with increasing shear rate. However,
beyond a certain shear rate value, the viscosity remains nearly con-
stant. This viscosity value is defined as the final viscosity. The final
viscosity is accepted as the instant apparent viscosity value of any mix
at a predefined shear rate (in this study, 30 s−1 ). At comparatively
high shear rates, most of the mixtures showed a stabilized tail of
viscosity curve. Because of this, the instant viscosity values calculated
by using the Herschel-Bulkley model at 30 s−1 were used for
comparison of the viscosity of different mixtures.
Mortar Mixture Test Methods
The flow value and V-funnel flow time of the mortar mixtures were
obtained in accordance with ASTM C1437 (ASTM 2013a) and
EFNARC (2005) standards, respectively, at 15-min time intervals
Period: 1 2 3 4
35
30
Shear rate (1/s)
25
20
15
10
5
0
0 30 60 90 120 150 180 210 240 270 300 330 360 390
Time (s)
Fig. 2. Shear rate history applied for investigation of the rheological
parameters of the mixtures
© ASCE
J. Mater. Civ. Eng., 2017, 29(8): 04017066
up to 60 min. The dynamic and static yield stress and final viscosity
of the mortar mixtures was determined similar to those of the paste
mixtures. The compressive strength of mortar mixtures was deter-
mined in accordance with ASTM C190 (ASTM 2013b) on 50-mm
cube specimens.
Concrete Mixtures Test Methods
The slump value and air content of the fresh concrete were determined
in compliance with EN 12350-2 (CEN 2010c) and ASTM C 231
(ASTM 2003) standards, respectively. The loss in consistency of
the concrete mixtures was measured at time intervals of 15 min,
up to 60 min. The unit weight of the concrete mixtures both in
fresh and hardened states were determined in accordance with EN
12350-6 (CEN 2010d) and EN 12390-7 (CEN 2010e) standards, re-
spectively. The strength of the concrete mixture was obtained accord-
ing to EN 12390-3 (CEN 2010b) on 100-mm cube specimens.
XRD Analysis
A Rigaku D/Max-2000/PC (Tokyo, Japan) model Cuk α XRD ana-
lyzer was used. Measurements were conducted at 40 kilovolts (kV)
under 36 milliamps (mA) current. Scanning intervals were 2θ ¼
8–10°C with a speed of 2°=min. X-ray diffraction analysis was per-
formed on 6-h-old cement paste samples having a W/C ratio of 0.35
and containing three different cement types. The specimens were
dried in an oven at 40°C for 12 h before testing. The dried samples
were crushed and sieved through No. 325 (45 μm) sieve. The
material passing No. 325 sieve was used in XRD analyses.
Test Results and Discussion
Fresh Properties of the Mixtures
Marsh-funnel flow time, miniflow, and temperature of the mixtures
containing C5.85 , C2.77 , and C1.90 cement types with different C3 A
contents are demonstrated in Fig. 3 and Table 7. The results show
that Marsh-funnel flow time of the mixtures decreased by increasing
their HRWR admixture content. However, beyond a certain level
(saturation point), the increase in admixture content did not have a
major effect on the flow time of the mixture. Irrespective of the
C3 A content of the cement, saturation point of the mixtures was found
to be 1.25 wt.% of cement. However, lower Marsh-funnel flow times
110 C5.85 paste mixture
C2.77 paste mixture
100 C1.90 paste mixture
Marsh-funnel flow time (sn)
90 W/C ratio = 0.35
T = 22oC
80
70
Saturation point
60
50
40
30
20
0.5 0.75 1 1.25 1.5 1.75 2 2.25
Admixture/cement ratio(%)
Fig. 3. Marsh-funnel flow time values of paste mixtures containing
various amounts of admixture
04017066-4 J. Mater. Civ. Eng.
 Table 7. Marsh-Funnel Flow Time, Minislump, and Temperature Values of Paste Mixtures
Admixture/cement ratio (%)
Property Mixture 0.75 1 1.25 1.5 1.75 2 2.25 2.5
Flow time, s C5.85 mixture 109.3 60 46.2 44.5 41.8 41.4 40.3 40.5
C2.77 mixture 55.3 39.5 35.4 32.5 31.8 30.1 29.4 29.8
C1.90 mixture 48.3 39.2 32.31 30.3 28.8 28.2 26.4 29.1
Mini-slump, mm C5.85 mixture 150 170 175 180 180 175 180 Segregated
C2.77 mixture 170 175 180 180 180 180 180 Segregated
C1.90 mixture 175 175 180 180 185 185 190 Segregated
Temperature, C° C5.85 mixture 27.7 27.6 26.9 27.8 27 27.5 27.6 27.8
C2.77 mixture 27.3 26.7 26.5 26.5 26.9 26.7 26.1 26.0
C1.90 mixture 27.9 26.6 26.3 26.3 26.8 26.5 26.1 26.1
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in the saturation point was obtained in the mixtures containing ce-
ment with lower C3 A contents, i.e., upon increasing the C3 A content
of the cement from 1.90 to 2.77 and 5.88%, Marsh-funnel flow time
of the mixtures increased by 30 and 43%, respectively.
Minislump values of the paste mixtures increased with the in-
crease in admixture content (Table 7). However, minislump values
of the mixtures were fixed beyond a certain admixture content. When
the admixture content was increased to 2.5%, the mixtures segre-
gated, thus, no Marsh-funnel or minislump value was measured.
Conversely, in the mixture containing 0.75 wt.% of the cement
HRWR admixture, there was a 15% increase in minislump when
the cement C3 A content was reduced from 5.58 to 1.90%. However,
this difference decreased with increasing dosage of admixture. Be-
yond a certain admixture content there was no change in minislump
value of the mixtures. Test results showed that the temperature of
mixtures did not change with the increase in admixture dosage.
Nevertheless, it increased slightly with the increase in cement C3 A
content.
To determine the rheological characteristics of the mixtures,
their shear stress-shear rate and shear stress-time diagrams were
plotted. For instance, shear stress-shear rate and shear stress-time
diagrams of C5.85 paste mixture having a 0.32 W/C ratio and con-
taining different amounts of HRWR admixture are shown in Figs. 4
and 5, respectively. The dynamic and static yield stresses and final
viscosity obtained from shear stress-shear rate and shear stress-time
diagrams are given in Table 8.
It can be understood from the shear stress-shear rate graph that
the flow curve of the paste mixtures was compatible with the
Herschel-Bulkley model governed by Eq. (1)
τ ¼ τ o þ b:γ̇ p ð1Þ
where b and p are defined as Herschel-Bulkley consistency coef-
ficient and Herschel-Bulkley index, respectively. Table 8 shows all
of the mixtures had a P value less than 1, indicating their pseudo-
plastic (deformation softening) behavior (Koehler and Fowler
2004). In addition, upon increasing the admixture content, the flow
curves fitting models of the mixtures became more compatible with
the experimental values.
When the W/C ratio increased from 0.32 to 0.35, dynamic and
static yield stresses and final viscosity values of the paste mixtures
reduced, indicating improvement in the rheological properties of
the mixtures (Table 9). Table 9 shows that in the paste mixtures

Fig. 4. Shear stress-viscosity relation of paste mixture containing cement C5.85 with a W/C ratio of 0.32

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Fig. 5. Time-dependent shear stress change of paste mixture containing cement C5.85 with a W/C ratio of 0.32

Table 8. Rheological Properties Results of Paste Mixtures Table 9. Reduction of Rheological Values (Decrease Percentage) upon
Increasing W/C Ratio from 0.32 to 0.35
Admixture dosage
(wt.% of cement) Admixture dosage (wt.% of
W/C
cement)
ratio Miximum Rheological properties 0 (%) 0.1 (%) 0.2 (%)
Mix Rheological properties 0 (%) 0.1 (%) 0.2 (%)
0.32 C5.85 a
Yield stress (Pa)
Dynamic 97.9 88 44.25 C5.85 Yield stress (decrease %)
Static 1,738 185.4 79.3 Dynamic 17 43 14
Final viscosity (Pa·s) 13.17 8.39 4.22 Static 83 44 29
Herschel-Bulkley index 0.85 0.77 0.54 Final viscosity (decrease %) 50 43 31
C2.77 Yield stress (Pa)
Dynamic 95.38 75.3 36.3 C2.77 Yield stress (decrease %)
Static 1,278 155.9 58.8 Dynamic 36 51 79
Final viscosity (Pa·s) 9.25 5.8 4.05 Static 88 59 79
Herschel-Bulkley index 0.71 0.53 0.42 Final viscosity (decrease %) 59 33 73
C1.90 Yield stress (Pa) C1.90 Yield stress (decrease %)
Dynamic 81.25 58.73 8.21 Dynamic 40 79 99
Static 461.6 63.5 11.96 Static 82 71 84
Final viscosity (Pa·s) 6.8 4.1 1.95 Final viscosity (decrease %) 26 72 88
Herschel-Bulkley index 0.54 0.40 0.33
0.35 C5.85 a Yield stress (Pa)
Dynamic 80.8 50.3 38.21 Table 10. Reduction of the Rheological Characteristics upon Increasing
Static 289 104.1 56.4 the Admixture Level from 0% to 0.2 wt.% of Cement
Final viscosity (Pa·s) 6.59 4.78 2.9
Herschel-Bulkley index 0.79 0.53 0.47 Mix
C2.77 Yield stress (Pa) W/C ratio Rheological properties C5.85 C2.77 C1.90
Dynamic 61.25 36.7 7.71
Static 155.6 63.9 12.5 0.32 Yield stress (decrease %)
Final viscosity (Pa·s) 3.75 3.9 1.11 Dynamic 55 62 89
Herschel-Bulkley index 0.60 0.48 0.42 Static 95 95 99
C1.90 Yield stress (Pa) Final viscosity (decrease %) 68 56 77
Dynamic 48.37 12.62 0.1 0.35 Yield stress (decrease %)
Static 81.7 18.5 1.86 Dynamic 52 87 99
Final viscosity (Pa·s) 5 1.15 0.23 Static 80 92 97
Herschel-Bulkley index 0.48 0.34 0.29 Final viscosity (decrease %) 55 70 95
a
It is designation of the mortar mixture prepared with cement containing a
ratio of 5.85% C3 A. enhancement in the rheological properties was better than that
of the mixtures without water-reducing admixture. As expected,
containing C5.85 cement, when the W/C ratio increased the rheo- the rheological properties of the mixtures were improved by using
logical properties of the mixtures containing no HRWR, admixture HRWR admixture. The effect was more pronounced in the mixtures
showed greater reduction than those of the mixtures containing containing higher amounts of the HRWR admixture.
HRWR admixture. The improvement in the rheological properties Table 10 shows the percent reduction of the rheological charac-
with increasing W/C ratio was lower in the mixtures containing teristics upon increasing the admixture level from 0 to 0.2 wt.% of
higher amounts of HRWR admixture. However, upon increasing cement. Table 10 shows that the C5.85 paste mixtures improvement
the W/C ratio in C1.90 paste mixtures containing HRWR admixture, in the rheological parameters was more obvious in the mixtures

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 350
350
C5.85 mortar mixture 300
330 320 280
C2.77 mortar mixture
305 305
310 250 230
C1.90 mortar mixture
Flow value (mm)

290 285

Flow value (mm)

280
270
280 200 210
270 280

245 265 185

250 260
255
250 150
230 215 220 235
205
225
210 200 100 C5.85 mortar mixture
205
190 190 C2.77 mortar mixture
180
190 50 C1.90 mortar mixture
170
0 0.1 0.2 0.3 0.4 0.5
Admixture dosage (%) 0
0 15 30 45 60
Fig. 6. Relationship between flow values of mortar mixtures and
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Time (min)
admixture dosage
Time (min) 0 15 30 45 60
C5.85 mixture 100 95 84 73 66
Relative flow
C2.77 mixture 100 98 86 80 75
value (%)
having a 0.32 W/C ratio. However, the reduction in rheological C1.90 mixture 100 100 91 86 82
parameters in the C1.90 paste mixtures after adding the admixture
was more obvious in the mixtures having 0.35 W/C ratio. Fig. 7. Time-dependent flow of mortar mixtures
It is known that any reduction in the dynamic and static yield
stress and final viscosity values is an indication of the improvement
in the rheological property of the mixture. Irrespective of the W/C 30
ratio and admixture content of the mix, using cement with lower 28.2
C3 A content improved the rheological characteristics of the paste. 25

V-funnel flow time (s)

When the C3 A content of the cement reduced from 5.85 to 1.90%,
the reduction in dynamic and static yield stresses and final viscosity
of the paste mixtures having a 0.32 W/C ratio and containing no
HRWR admixture were found to be 17, 73, and 48%, respectively.
The effect was more pronounced by increasing W/C ratios and
admixture content of the mixture.
The flow values of 24 different mortar mixtures containing 0 to
0.5% HRWR admixture were determined. Test results are shown in
Fig. 6. Among the mixtures without HRWR admixture, the C5.85
mixture showed minimum flow value. Compared with C5.85 mortar
mixture, C2.77 and C1.90 showed 5 and 12% higher flow values,
respectively. Irrespective of the C3 A content of the cement, the flow
values of all of the three series mixture increased with using the
admixture and increasing its content. However, for the same admix-
ture content, compared with the other two series, C1.90 mixture
showed the best flow performance. The flow value of the C5.85 ,
C2.77 , and C1.90 mixtures showed 55, 60, and 71% increase upon
increasing the admixture content from 0.2 to 0.5%. The flow of
C1.90 mixture containing 0.5% admixture was 15 and 25% more
than those of C2.77 and C5.85 mixtures, respectively.
To investigate the time-dependent flow changes, mortar mix-
tures having 280-mm flow value were prepared. The admixture re-
quirement for the given flow was 0.5% in C5.85 mixtures. It reduced
by decreasing the C3 A content of the cement, thus, the correspond-
ing values for C2.77 and C1.90 was 0.4 and 0.34%, respectively. The
flow values of the mixtures were measured at 15-min intervals up to
60 min. The change in flow values by elapsing time and the relative
flow values compared to the original flow value of each mix are
shown in Fig. 7.
As expected, the flow values of the mixtures reduced with time.
However, the C5.85 mixture showed the maximum flow loss after
60 min compared with the other mixtures. At the end of 60 min,
C5.85 , C2.77 , and C1.90 showed 34, 25, and 18% flow loss, respec-
tively. At the end of 60 min, the flow loss of the C1.90 mixture was
10 and 20% less than those of C2.77 and C5.85 , respectively.
To investigate the change in V-funnel flow time, the V-funnel
flow time of the three mortar mixtures having 280-mm flow value
were measured at 15-min intervals up to 30 min. However, the C5.85
20 21.4
15 14.1
11.2
10
C5.85 mortar mixture
8.3
C2.77 mortar mixture
5
C1.90 mortar mixture
0
0 15 30
Time (min)
Fig. 8. Time-dependent V-funnel flow time of mortar mixtures
mixture showed no flow after 15 min. Beyond 30 min, no flow was
recorded in the mixtures. Test results are shown in Fig. 8.
The initial V-funnel flow time of the C5.85 mixture was 25 and
70% longer than that of C2.77 and C1.90 mixtures, respectively. After
15 min, V-funnel flow time of the C1.90 mixture was 22% shorter
than that of C2.77 . Thus, C1.90 mixtures, having the lowest C3 A con-
tent, showed the best performance in terms of V-funnel flow time.
As noted previously, the rheological properties of the mortar
mixtures were determined by a similar method as the paste mix-
tures. For instance, shear stress-shear rate and shear stress-time dia-
grams of the mortar mixture with C5.85 cement type with a 0.5 W/C
ratio are shown in Figs. 9 and 10. The diagrams show that rheo-
logical behavior of the mortar mixtures was compatible with the
Herschel-Bulkley model. Dynamic and static yield stresses and
final viscosity values of the mixtures obtained from the figures are
summarized in Table 11.
Similar to the paste mixtures, the static yield stress, dynamic
yield stress, and final viscosity values of the mortar mixtures were
reduced by increasing the W/C ratio and/or admixture content. In
addition, concerning rheological behavior, the best and the worst
performances were observed in C190 and C5.85 mortar mixtures, re-
spectively. When the C3 A content of the cement reduced from 5.85
to 1.90%, dynamic and static yield stresses and final viscosity of the

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Fig. 9. Shear stress-viscosity relation of mortar mixture containing cement C5.85 with a W/C ratio of 0.5

Fig. 10. Time-dependent shear stress change of mortar mixture containing cement C5.85 with a W/C ratio of 0.5

mortar mixtures with a 0.5 W/C ratio and containing 0.3% HRWR
admixture decreased by about 60, 45, and 66%, respectively. The
effect of C3 A content of the cement on the rheological properties
of mortar mixtures was reduced by increasing the W/C ratio and
decreasing the admixture content.
The effect of cement C3 A content on fresh state properties of the
concrete mixtures was detected in mixtures having a slump value of
225
5 mm. For this purpose, 4.3 kg=m3 HRWR admixture was
used in the C5.85 concrete mixture. For the same slump, the admix-
ture requirement of C2.77 and C1.90 concrete mixtures was found to
be 5 and 16% lower than that of C5.85 mixtures. Air content, slump,
and flow values of the mixtures are shown in Table 6. Air contents
of the concrete mixtures showed negligible change with the cement
type. The change in slump and flow values of the concrete mixtures
by elapsing time are shown in Fig. 11. Slumps and flows of the
mixtures reduced with time as expected. Slump value of the C1.90
mixtures did not show a considerable change in the first 30 min.
This period was found to be only 15 min for the C2.77 and C5.85
mixtures. The C5.85 concrete mixture showed 86% slump loss after
45 min. This mixture showed no slump at the end of 60 min. How-
ever, C2.77 and C1.90 mixtures showed 71 and 60% of slump loss,
respectively, at the end of 60 min. Besides, C5.85 , C2.77 , and C1.90

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 Table 11. Rheological Properties of Mortar Mixtures
Admixture dosage (wt.% of cement)
W/C ratio Miximum Rheological properties 0 (%) 0.1 (%) 0.2 (%) 0.3 (%)
0.5 C5.85 a
Yield stress (Pa)
Dynamic — — 93.64 66.62
Static — — 1,177.4 937.6
Final viscosity (Pa·s) — — — 19.21
C2.77 Yield stress (Pa)
Dynamic — — 89.33 35.66
Static — — 979.2 691.6
Final viscosity (Pa·s) — — — 14.08
C1.90 Yield stress (Pa)
Dynamic — — 73.79 26.81
Static — — 882.04 519.8
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Final viscosity (Pa·s) — — 18.07 13.79

0.6 C5.85 a Yield stress (Pa)
Dynamic 88.57 30.80 — —
Static 997.1 422.4 — —
Final viscosity (Pa·s) 9.03 6.05 — —
C2.77 Yield stress (Pa)
Dynamic 57.87 24.26 — —
Static 741.6 309.6 — —
Final viscosity (Pa·s) 6.35 5.12 — —
C1.90 Yield stress (Pa)
Dynamic 45.54 15.87 — —
Static 514.9 240.1 — —
Final viscosity (Pa·s) 6.08 4.51 — —
a
It is designation of the mortar mixture prepared with cement containing a ratio of 5.85% C3 A.

C5.85 concrete mixture

mixtures showed 46, 29, and 21% of flow loss at the end of the first
250 230 230
30 min. No flow was measured in C5.85 mixtures after 45 min.
C2.77 concrete mixture
200 200 Nevertheless, C2.77 and C1.90 mixtures had 240 and 280-mm flow
200 180 C1.90 concrete mixture value, respectively, at the end of the same period. According to
Slump value (mm)

150 test results, the best and the worst performances of the concrete
150 130 mixtures in terms of fresh state properties was found in the C1.90
120
and C5.85 mixtures. In addition, Fig. 11 shows that in all of the con-
100
90 crete mixtures, flow loss was more pronounced than slump loss, par-
60 ticularly in the mixtures containing cement with high C3 A content.
50
Test results indicated that all of the fresh cementitious systems
30
containing C5.85 cement showed the lowest performance. This arises,
0 in part, from the higher C3 A content of this cement and, in
0
15 30 45 60 part, because its higher fineness compared with the other cements (Ta-
(a)
ble 1). According to the literature, high C3 A content of the cement
Time (min)
adversely affects the fresh and rheological behavior of the cementi-
tious systems (Perenchio et al. 1979; Aïtcin 2004). The fact is attrib-
C5.85 concrete mixture uted to the formation of a high amount of needle-like ettringite crystals
500 460 C2.77 concrete mixture
440 that consume a considerable amount of the mixing water, resulting in
450 C1.90 concrete mixture
400 a decrease in the workability of the cementitious system (Tagnit-
380
400
350
Hamou and Aïtcin 1993; Prince et al. 2002). X-ray diffraction analysis
Flow value (mm)

350 of the paste mixtures containing three different cements are shown in
300
280 Fig. 12. The phase analysis demonstrated the presence of ettringite in
260
240 all of the paste mixtures. However, higher intensity of the ettringite
250
peak in C5.85 mixture is an indication of its larger amount in this mix-
200 ture. However, in the presence of water-reducing admixture in the
150 system, the admixture prevents flocculation of the cement by electro-
100 static repulsion. In addition, the admixture slows down the hydration
50
of C3 A compound by covering its surface. Thus, the workability of
0 0 0 0 the cementitious system improves upon retardation of ettringite for-
0
15 30 45 60
mation (Vernet and Noworyta 1992; Ramachandran 1995). According
to other researchers, as a result of the presence of the water-reducing
(b) Time (min) admixture, the massive ettringite with a cubic crystalline structure,
which is less harmful to the fresh state properties of the system, occurs
Fig. 11. Change in (a) slump; (b) flow values of concrete mixtures by
instead of the needle-like ettringite crystals (Bassant 1994; Prince et al.
elapsing time
2003). In this study, enhancement in the fresh properties of the paste

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 researchers (Alonso and Puertas 2015). The high specific surface
area of ettringite arising from the presence of polycarboxylate ether–
based admixture is reported to be responsible for this fact. Thus,
performance of the admixture is reduced and, accordingly, the fresh
properties of the mixtures is affected negatively (Dalasa et al.
2015).

Compressive Strength
The effect of cement C3 A content on the compressive strength de-
velopment of either mortar or concrete mixtures was determined on
mortar mixtures having a flow value of 280 mm and concrete mix-
tures with a slump value of 225
5 mm. The admixture content of
the mixtures varied by the C3 A content of cement. The results ob-
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tained on 1, 3, 7, and 28-day age specimens are given in Figs. 13

and 14, respectively. In general, 1-day and 3-day strength of the
mixtures increased considerably by increasing cement C3 A con-
tent. The effect of C3 A content of cement on the strength of the
mixtures diminished at later ages. One-day compressive strength
of the mixtures was significantly affected by the calcium sulfoalu-
minates. However, the later age strength of the mixtures was con-
trolled primarily by calcium silicate hydrate (Mehta and Monteiro
2006; Neville 2010). In addition, C3 A content of the cement was
found to be more effective on the strength of the mortar mixture
than on the strength of concrete mixtures. Not surprisingly, the mix-
tures that showed higher flow loss or slump loss also showed higher
early strength values.

Fig. 12. XRD patterns of cement pastes containing different cement
types, 2θ ¼ 8–10°C [Ettringite: Ca6Al2(SO4)3(OH)12.26H2O]
mixtures was observed with 0.2 wt.% of cement HRWR
admixture. However, HRWR admixture was more effective in the
C1.90 mixture than the other two mixtures containing cements with
higher C3 A contents. The same results were reported by other
Conclusion
The following conclusions were drawn for the materials used and
tests applied in this study:
By lowering the C3 A content of the cement
• Saturation point of the HRWR admixture showed no change.
However, Marsh-funnel flow times and minislump values of
the paste mixtures reduced;
• Rheological properties (dynamic and static yield stresses and
final viscosity) of the paste and mortar mixtures were enhanced;

C5.85 mortar mixture C2.77 mortar mixture

Ç1.90 mortar mixture C5.85 mortar mixture-relative strength
C2.77 mortar mixture-relative strength C1.90mortar mixture-relative strength
90 103
101

80 100 100
90
96 92
Relative compressive strength (%)
Compressive strength (MPa)

70 89
80
76
60

50 60
59

40
40
30

20
20
10

0 0
1-day 3-day 7-day 28-day

Fig. 13. Compressive strength of mortar mixtures and relative compressive strength compared with C5.85 mortar mixture

© ASCE 04017066-10 J. Mater. Civ. Eng.

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 C5.85 concrete mixture C2.77 concrete mixture
C1.90 concrete mixture C5.85 concrete mixture-relative strength
C2.77 concrete mixture-relative strength C1.90 concrete mixture-relative strength

90 104

80
100 100
91 98
93

Relative compressive strength (%)

Compressive strength (MPa)
93
70 85 90
80 80
60

50 60
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40
40
30

20
20
10

0 0
1-day 3-day 7-day 28-day

Fig. 14. Compressive strength of concrete mixtures and relative compressive strength compared with C5.85 concrete mixture

• Admixture requirement of the mortar mixtures for a given flow
were reduced;
• Flow and V-funnel flow time retention of the mortar mixtures
improved and V-funnel flow time was reduced;
• Slump-flow values and consistency retention potential of the
concrete mixtures increased; and
• The early strength of either mortar or concrete mixtures reduced.
The effect was negligible at later ages.
Irrespective of the cement C3 A content
• The rheological behavior of either paste or mortar mixture
was compatible with the Herschel-Bulkley model. The degree
of compatibility increased with the presence of admixture and
increasing its content;
• The static yield stress of the mixtures was found to be greater
than their dynamic yield stress. The difference between those
reduced by the utilization of admixture and by increasing its
amount; and
• A strong linear relationship between dynamic yield stress-
minislump values in the paste mixtures and dynamic yield
stress-flow values in the mortar mixtures were observed.
Acknowledgments
The authors would like to thank Oyak Cement plant for their kind
assistance in providing the cement and determining the chemical
composition of the cement. The first author would like to acknowl-
edge the scholarship provided by Turkish Cement Manufacturers
Association during his Ph.D. study.
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