Cite this article Research Article

Özen S, Altun MG, Mardani-Aghabaglou A and Ramyar K Paper 2100134

Multi-effect of superplasticisers main and side-chain length on cementitious systems with fly Received 02/06/2021;
ash. Accepted 26/11/2021
Magazine of Concrete Research,
https://doi.org/10.1680/jmacr.21.00134 ICE Publishing: All rights reserved

Magazine of Concrete Research

Multi-effect of superplasticisers main and

side-chain length on cementitious systems
with fly ash
&
1 Süleyman Özen &
3 Ali Mardani-Aghabaglou
Assistant Professor, Department of Civil Engineering, Faculty of Associate Professor, Department of Civil Engineering, Faculty of
Engineering and Natural Sciences, Bursa Technical University, Yildirim- Engineering, Bursa Uludag University, Nilüfer-Bursa, Turkey
Bursa, Turkey (Orcid:0000-0001-5522-427X) (corresponding author: (Orcid:0000-0003-0326-5015)
suleyman.ozen@btu.edu.tr) &
4 Kambiz Ramyar
&
2 Muhammet Gökhan Altun Professor, Department of Civil Engineering, Faculty of Engineering,
Civil Engineer, Bursa Metropolitan Municipality, Osmangazi-Bursa, Ege University, Bornova-Izmir, Turkey (Orcid:0000-0003-2200-2691)
Turkey (Orcid:0000-0002-7952-1882)

1 2 3 4

In this study, the effect of main and side chain lengths of polycarboxylate ether-based high-range water-reducing
admixtures (WRAs) on the fresh properties, compressive strength and water absorption of cementitious systems
containing 0, 15, 30 and 45 wt% fly ash was investigated. For this purpose, three WRAs with the same molecular
weight but different chain lengths were produced. According to the test results, the flowability of the paste and
mortars was negatively affected when the length of the main and side chains of the admixture was longer or shorter
than a certain value. This adverse effect is thought to arise from weakening of the adsorption of the admixture with
an increase in its chain lengths. However, when the main and side chain lengths of the admixture were shorter or
longer than a certain value, the time-dependent flow properties of the mortar mixtures improved. The main and side
chain lengths of the WRAs did not have a significant effect on the compressive strength and water absorption
capacity of the mortar mixtures. However, irrespective of the admixture characteristics, with an increase in fly ash
substitution, the flow and time-dependent flow properties of the mixtures were negatively affected but their water
absorption decreased.

Keywords: admixture/compressive strength/flowability

Notation Introduction
Ed dynamic elasticity modulus of self-compacting concrete The comb-shaped structure of a water-reducing admixture
Mn number-average molecular weight (WRA) consists of two parts. The first part comprises anionic
Mw weight-average molecular weight functional groups and the other consists of polyethylene oxide
m mass of cement side chains (Hanehara and Yamada, 2008; Tsubakimoto et al.,
Q adsorption amount (mg/l) of polycarboxylate ether on 1984). There are two main synthetic approaches in the pro-
cement duction of polycarboxylate-based admixtures. One approach
Tc total organic carbon concentration of cement solution involves the free radical copolymerisation of a monomer
T0 total organic carbon concentration of polycarboxylate bearing carboxylic groups and another monomer bearing a
ether solution before adding cement side chain. This method is the most widely used in the indus-
T1 total organic carbon concentration of polycarboxylate try, because of its simplicity and cost-effectiveness.
ether solution when polycarboxylate ether is at the Furthermore, radical copolymerisation is an ideal approach for
adsorption equilibrium on the surface of the cement introducing different types of monomer into the main chain.
particles With this approach, the admixture has a gradient distribution
V volume of polycarboxylate ether solution of side chains along the main chain. Another approach is
w total organic carbon concentration per unit mass of polymer analogue esterification or amidation of carboxylic
polycarboxylate ether groups bearing a backbone with monofunctional polyethylene

1
Magazine of Concrete Research
Figure 1. Structure of WRA (Aïtcin and Flatt, 2016)
glycol. In this approach, admixtures with narrower structural
distributions and lower molecular weights can be produced,
owing to the constant length of the main chain. At the same
time, this approach provides a uniform distribution of the side
chains along the main chain (Aïtcin and Flatt, 2016).
The admixtures thus produced are referred to as polycarboxy-
late ether (PCE), polycarboxylate ester or polycarboxylate. As
shown in Figure 1, the structure of the WRA generally consists
of a main chain or backbone, to which the non-ionic polyethy-
lene oxide side chains are grafted. The main chain also con-
tains carboxylic functional groups. The carboxylic groups on
the main chain of the admixture impart a negative charge to
the main chain. The negatively charged main chain is respon-
sible for the adsorption of the admixture on the positively
charged cement particles. The dispersion ability of the admix-
ture in solution depends on its side chains forming steric
effects. Adsorption is largely dependent on the number of car-
boxylic groups, while the steric effect depends on the amount
and length of the side chains of the adsorbed polymer (Flatt
et al., 2009; Nawa et al., 2000). Accordingly, the combined
effects of anionic monomers and side chains in WRAs deter-
mine the dispersive effect of the admixture in the cementitious
system. In this context, it is important to understand the effect
of anionic groups and non-ionic side chains on the fresh and
hardened state properties of cementitious systems.
The chemical structure, anionic monomer type, molecular
weight, main chain length, anionic/non-ionic group ratio,
number, density and length of side chains of the WRA signifi-
cantly affect the properties of cementitious systems. In recent
years, the aim has been to increase the chemical admixture
efficiency by revising these parameters (Li et al., 2005;
Mardani-Aghabaglou, 2016; Mardani-Aghabaglou et al.,
2017a, 2017b; Ran et al., 2009). According to the studies, the
2
Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar
Anionic functional group
(anionic monomer)
Main chain
Side chain
adsorption characteristics of the admixture improves by
decreasing the side chain length, which leads to a decrease in
the steric effect. As the main chain length increases, the
number of anionic functional groups increases and thus the
electrostatic effect increases (Borsoi et al., 1999; Bouhamed
et al., 2007; Plank and Hirsch, 2007; Schober and Flatt, 2006).
In the study conducted by Yamada et al. (2007), the use of
admixtures with long side chains and short main chains
improved the flow of paste mixtures. In paste mixtures contain-
ing admixtures with long side chains, the setting time was
short and flow loss was rapid. Conversely, it was stated that
long main chains did not affect the time-dependent fluidity but
increased the setting time of the mixtures slightly. In another
study by Qiu et al. (2011), it was found that the dispersive
effect of admixtures having both short and long side chains
was better than that of admixtures with only short or only
long side chains. Furthermore, the retarding effect of admix-
tures with short side chains was reported to be greater than
that of admixtures with long side chains. Matsuzawa et al.
(2019) investigated the effect of the main chain length of
WRAs on their adsorption property, and emphasised that the
admixture’s adsorption properties are related to the main chain
length and the distance between particles. It was explained that
admixtures with short main chains can penetrate the cement
particles and help to disperse the particles. Conversely, admix-
tures with a long main chain can interact with several particles
at the same time and lead to a bond bridge between them, par-
ticularly when the distance between the cement particles is
very small, as is the case in low water/powder ratio mixtures.
In addition to chemical admixtures, some mineral additives,
such as fly ash, are used to increase the pumpability, workabil-
ity and durability of cementitious systems. Especially in self-
compacting concretes, owing to its spherical morphology, fly
ash is preferred to obtain a cohesive mixture, although some
Magazine of Concrete Research
fly ashes may increase the water requirement of the mixture
(Mardani-Aghabaglou, 2016). With the use of fly ash, which is
a waste product of thermal power plants, in concrete mixtures,
in addition to the improvement in concrete properties, many
economic and environmental gains – such as reduction of
cement and consequent energy consumption, reduction of
carbon dioxide (CO2) emission and preservation of natural
resources – can be achieved (De Lena et al., 2019). The effect
of using fly ash as fine aggregate on the mechanical and flow
properties, unit weight and ultrasonic pulse velocity of mortar
mixtures was investigated by Bilir et al. (2015), who reported
that the flow performance of the mixtures decreased with the
increase in fly ash utilisation ratio. In an experimental study
conducted by Moghaddam et al. (2019), the effect of fly ash
fineness on the hydration heat, microstructure, flow and com-
pressive strength of paste mixtures was investigated. In this
context, 0, 20 and 40 wt% of cement was replaced by fly ashes
of three different finenesses (obtained from the same power
plant). Paste mixtures with a water/binder ratio of 0.4 were
produced. According to the results, the heat of hydration of
the mixtures could be decreased by increasing the fly ash fine-
ness and increasing its utilisation rate. Furthermore, the
increase in fly ash fineness positively affected both the flow
performance and the compressive strength of the mixture.
In summary, there are studies in the literature on the effect of
admixture chain length on the fresh properties of cementitious
systems. However, the molecular weights of the polymers vary,
depending on the lengths of the main and side chains of the
admixture. Moreover, the majority of the admixtures used to
study cement–admixture compatibility are commercial pro-
ducts. Admixture manufacturers generally do not share the
basic properties of their products, as these are trade secrets.
Therefore, comparison and evaluation of the test results
becomes difficult, owing to the differences between the physical
and chemical characteristics of the admixtures, as well as the
difference between the raw materials of the polymers. In this
study, the lengths of the main and side chains were changed,
keeping the molecular weights of the admixtures constant. The
effects of admixtures synthesised in this way on some fresh and
hardened state properties of cementitious systems were
Table 1. Physical and mechanical properties and chemical composition of cement
Item Content: %
SiO2 18.86
Al2O3 5.71
Fe2O3 3.09
CaO 62.70
MgO 1.16
SO3 2.39
Na2O + 0.658 K2O 0.92
Cl− 0.01
Insoluble residue 0.32
Loss of ignition 3.20
Free CaO 1.26
Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar
investigated. In addition, cement paste and mortar mixtures
containing 0, 15, 30 and 45 wt% fly ash were prepared to
investigate the compatibility of the admixtures with fly ash
cementitious systems.
Experimental study
Materials
In this study, a CEM I 42.5 R cement conforming with stan-
dard TS EN 197-1 (TSE, 2012) and a siliceous fly ash comply-
ing with standard TS EN 450-1 (TSE, 2013a) were used. The
chemical composition, physical properties and mechanical
properties of cement and fly ash are given in Tables 1 and 2,
respectively. As for aggregate, standard sand in accordance
with standard TS EN 196-1 (TSE, 2016) was used. The
specific gravity and water absorption capacity of standard sand
were determined as 2.72 and 0.7%, respectively, in accordance
with standard TS EN 1097-6 (TSE, 2013b).
PCE characterisation
The WRAs were characterised by means of Fourier transform
infrared (FTIR) spectroscopy and gel permeation chromato-
graphy (GPC) according to the study of Özen et al. (2020).
The FTIR spectra of admixtures are shown in Figure 2. The
molecular weights and polydispersity indices (PDIs) deter-
mined by the GPC analysis and chromatographs of the PCEs
are shown in Tables 3 and 4 and Figure 3, respectively. In
addition, the density, solid content, pH and viscosity of the
WRAs are given in Table 5.
The admixtures used in this study are designated by their main
and side chain lengths. For example, the admixtures with 17k,
21k and 40k main chain lengths and 1000, 2400 and
3000 g/mol side chain lengths are named PCE17k-3000,
PCE21k-2400 and PCE40k-1000, respectively.
The molecular weight, free non-ionic group content and
anionic/non-ionic group ratio of the admixtures were kept con-
stant at 48 kg/mol, 2.78 mol and 3.47, respectively. The main
chain length of the admixtures was optimised to contain an
average of 17, 21 and 40 non-ionic groups on each main chain.
Physical or mechanical property Value
Specific gravity 3.15
Residual on 0.045 mm sieve: % 7.6
Blaine specific surface: cm2/g 3530
Compressive strength, 1 day: MPa 14.7
Compressive strength, 2 days: MPa 26.8
Compressive strength, 7 days: MPa 49.8
Compressive strength, 28 days: MPa 58.5
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Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

Since the molecular weight and the anionic/non-ionic group In the first phase of this study, three control paste mixtures
ratio were kept constant, the number of anionic groups on the containing Portland cement and WRAs with three different
main chain of the admixture was proportional to the number chain lengths were prepared. In the second phase, nine paste
of non-ionic groups (Özen et al., 2020). mixtures, in which 15, 30 and 45 wt% of cement was substi-
tuted by fly ash, containing three different admixtures, were
produced. Thus, a total of 12 paste mixtures were tested. The
Mix proportions proportions of the mixtures and their designations are given in
Considering the studies reported in the literature, the Table 6. Designations of the paste mixtures was given in
water/binder ratio of the pastes, as determined using Marsh accordance with their admixture type and fly ash content. For
funnel and mini slump tests, was fixed at 0.35 (Aïtcin, 2004). instance, the paste mixtures including 21k WRA without fly
ash was named PC21k-2400-FA0. The mixture including the
same WRA (21k) and 30% fly ash by cement weight was
Table 2. Physical and mechanical properties and chemical compo-
sition of fly ash named PC21k-2400-FA30. Six different quantities of high-
range WRA in the range of 0.75–2 wt% of cement were used
Physical or in 12 paste mixtures to measure their Marsh funnel flow times
Item Content: % mechanical property Value
and mini flow values.
SiO2 59.22 Specific gravity 2.31
Al2O3 22.86 Blaine specific surface: 4300 A total of 12 different series of mortar mixtures similar to the
cm2/g
paste mixtures were prepared in accordance with standard
Fe2O3 6.31 Residual on 0.045 mm 10
sieve:% ASTM C109 (ASTM, 2021). Water/binder, sand/binder ratios
CaO 3.09 Strength activity index, 85.9 and flow of the mortars mixtures were fixed at 0.485, 2.75 and
7 days: % 270 ± 20 mm. Proportions of the mortar mixtures are pre-
MgO 1.31 Strength activity index, 100.7 sented in Table 7. The designations of the mortars were similar
28 days: %
to those of the pastes.
SO3 0.17 Strength activity index, 110.2
90 days: %
Na2O + 0.658 K2O 1.4 Test methods
Cl− 0.001 The adsorption amount of PCE on cement was determined
Insoluble residue 0.32
Loss of ignition 3.2
using a method similar to that used in the study of Altun et al.
Free CaO 0 (2020). The amount of PCE adsorption was determined by
using a total organic carbon (TOC) analyser. The adsorption
amount can be calculated as

ðT0 þ TC  T1 ÞV =w
Q¼
m

2918 PC17k-3000
where Q is the adsorption amount (mg/l) of PCE on cement,
1645

3378
PC21k-2400 T0 is the TOC concentration (mg TOC/l) of the PCE solution
1087
before adding cement, TC is the TOC concentration (mg
PC40k-1000
TOC/l) of the cement solution, T1 is the TOC concentration
4500 4000 3500 3000 2500 2000 1500 1000 500 0
(mg TOC/l) of the PCE solution when PCE is at the adsorp-
Wavenumbers: cm–1 tion equilibrium on the surface of the cement particles, V is
the volume (l) of the PCE solution, w is the TOC concen-
Figure 2. Fourier transform infrared spectra of polycarboxylate- tration per unit mass (mg TOC/mg PCE) of PCE and m is the
ethers mass (g) of cement (Li et al., 2005).

Table 3. Gel permeation chromatography analysis results of WRAs

Type of anionic Anionic/non-ionic Free non-ionic Molecular Main chain Side chain molecular
Admixture monomer group ratio: mol/mola group: mola weight: kg/mol lengtha weight: g/molb

PC40k-1000 Carboxylate 3.47 2.78 48 40k 1000

PC21k-2400 Carboxylate 3.47 2.78 48 21k 2400
PC17k-3000 Carboxylate 3.47 2.78 48 17k 3000

a
Calculated from gel permeation chromatography analysis, given as coefficients.
b
The side chains of the admixtures are polyethylene oxide. The molecular weight of side chain of the admixtures is related to its length.

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Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

Table 4. Mw, Mn and polydispersity indices of WRAs Table 6. Mix proportions of paste mixtures
Mw: Mn: Polydispersity index Cement: Fly Water: Admixture:
Admixture g/mol g/mol (Mw/Mn) Mixture g ash: g g %

PC40k-1000 47838 23401 2.04 PC40k-1000-FA0 700 — 245 0.75–2

PC21k-2400 47742 23836 2.00 PC21k-2400-FA0 700 — 245 0.75–2
PC17k-3000 47794 30173 1.58 PC17k-3000-FA0 700 — 245 0.75–2
PC40k-1000-FA15 595 105 245 0.75–2
PC21k-2400-FA15 595 105 245 0.75–2
PC17k-3000-FA15 595 105 245 0.75–2
PC40k-1000-FA30 490 210 245 0.75–2
150 PC21k-2400-FA30 490 210 245 0.75–2
PC17k-3000-FA30 490 210 245 0.75–2
100
PC40k-1000-FA45 385 315 245 0.75–2
Refractive index: a.u.

50 PC21k-2400-FA45 385 315 245 0.75–2

PC17k-3000-FA45 385 315 245 0.75–2
0
0 5 10 15 20 25 30 35 40
–50 Time: min

–100
PCE40k-1000 1000 to 3000 g/mol. This results in a slight decrease in the
–150 PCE21k-2400 adsorption of the admixture. However, the adsorption amount
PCE17k-3000
–200 increased considerably with decreasing admixture main chain
length, from 21k to 17k.
Figure 3. Gel permeation chromatographs of polycarboxylate-
ethers
Fresh state properties of cement paste mixtures
Marsh funnel flow times of the cement paste mixtures having
Table 5. Properties of WRAs admixtures with constant molecular weight and different chain
Density: Solid Viscosity at lengths are shown in Figure 4 and Table 9. The admixture
Admixture g/cm3 content: % pH 20°C: cps content of 0.75 wt% of the binder was insufficient for flow of
the pastes through the Marsh funnel. Thus, the admixture
PC40k-1000 1.15 48.1 3.94 460
PC21k-2400 1.12 59.9 4.02 1050 dosage of the pastes was kept between 1% and 2% in the
PC17k-3000 1.13 55.0 4.08 650 Marsh funnel test.

As can be seen from Figure 4, the admixture saturation point

for all of the binder–admixture pairs was determined as 1.5%,
Marsh funnel and mini slump experiments were carried out in
regardless of the admixture type and fly ash substitution level.
accordance with the methods proposed by Aïtcin (2004) and
The use of admixtures beyond the saturation point increases
Kantro (1980), respectively. The flow and flow loss of the
the risk of segregation and is also not economical (Aïtcin,
mortar mixtures at time intervals of 15 min up to 1 h were
2004; Mardani-Aghabaglou et al., 2017a, 2017b).
determined in accordance with ASTM C1437 (ASTM, 2020).
The mini V funnel test proposed by EFNARC (2002) was per-
Admixture PC40k-1000, having a longer main chain but
formed to measure the flow time of the mortar mixtures. The
shorter side chain than the PC21k-2400 admixture, was
compressive strengths of the mortar mixtures at five different
expected to show a greater adsorption than PC21k-2400. In
ages in between 1 and 90 days were determined on 50 mm
accordance with the results of TOC analysis given in Table 8,
cube specimens in accordance with the ASTM C109 standard.
the adsorption of PCE40k-1000 admixture (0.829 mg/g) is
Water absorption tests were conducted on 28 and 90 day
slightly higher than that of the PCE21k-2400 (0.814 mg/g).
mortar specimens in accordance with standard ASTM C642
The flow performance of the PC40k-1000-FA0 mixture was
(ASTM, 2016). All of the 252 mortar specimens prepared in
expected to be better than that of the PC21k-2400-FA0
this study were removed from the moulds after 24 h and cured
mixture; however, the opposite result was obtained. This nega-
until the testing day in lime-saturated water at a temperature
tive effect is thought to arise for two reasons: (1) the side
23 ± 2°C.
chains of the PC40k-1000 admixture were too short to create a
sufficient steric hindrance effect, and (2) the main chain of the
Results and discussion
PC40k-1000 admixture is long enough to intertwine with the
Adsorption side chains of nearby molecules. As stated in the literature,
The amounts of admixtures adsorbed on cement grains are while the adsorption performance of the admixture improves
given in Table 8. When the length of the main chain decreased with a reduction in the length of the side chain, the steric hin-
from 40k to 21k, the length of the side chain increased from drance effect becomes weaker. As can be seen from Table 3,

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Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

Table 7. Proportions of mortar mixtures

Mixture Cement: g Fly ash: g Water: g Sand: g Admixture ratio: %

PC40k-1000-FA0 500 — 242.5 1375 0.80

PC21k-2400-FA0 500 — 242.5 1375 0.60
PC17k-3000-FA0 500 — 242.5 1375 0.60
PC40k-1000-FA15 425 75 242.5 1375 0.70
PC21k-2400-FA15 425 75 242.5 1375 0.56
PC17k-3000-FA15 425 75 242.5 1375 0.56
PC40k-1000-FA30 350 150 242.5 1375 0.60
PC21k-2400-FA30 350 150 242.5 1375 0.50
PC17k-3000-FA30 350 150 242.5 1375 0.50
PC40k-1000-FA45 275 225 242.5 1375 0.50
PC21k-2400-FA45 275 225 242.5 1375 0.46
PC17k-3000-FA45 275 225 242.5 1375 0.46

Table 8. Amounts of WRAs adsorbed on cement particles
Admixture Amount of adsorption (mg/g cement)
PCE40k-1000 0.829
PCE21k-2400 0.814
PCE17k-3000 0.937
the number of anionic functional groups of the admixture
increases with the elongation of its main chain. Accordingly,
the electrostatic effect is expected to increase, but the opposite
happened. The interaction of the admixture with cement was
limited and its adsorption weakened, owing to interlacing of
the long main chains (Borsoi et al., 1999; Bouhamed et al.,
2007; Plank and Hirsch, 2007; Schober and Flatt, 2006).
Among the mixtures prepared in this study, the mixture con-
taining PC17k-3000 admixture showed the worst performance
with regard to Marsh funnel flow, owing to the intertwining of
the side chains, destruction of the polymer film layer and the
small electrostatic effect of the short main chains. Similar
effects were reported in other studies. As can be seen from the
TOC analysis results shown in Table 8, the adsorption amount
of the PCE17k-3000 admixture was the largest, compared with
the other admixtures. However, the Marsh funnel flow of the
mixture containing this admixture was low. The fact that the
admixture has a short main chain causes the amount of
anionic functional groups on the main chain to decrease and,
consequently, a weakening of the electrostatic effect (Ferrari
et al., 2011; Mardani-Aghabaglou et al., 2013; Peng et al.,
2013; Plank and Sachsenhauser, 2006; Qiu et al., 2011; Wang
et al., 2018).
Regarding the Marsh funnel flow of the pastes, the optimum
side chain length (molecular weight) and main chain length
were found to be 2400 g/mol and 21k, respectively. The Marsh
funnel flow values of the pastes at the admixture saturation
point were reduced by the fly ash inclusion, irrespective of the
WRA type. In other words, there was an increase in the
viscosity of the paste mixtures with the addition of fly ash.
This effect became more pronounced with the increase in fly
ash substitution level. This fact seems to arise from the higher
fineness and lower specific gravity of the fly ash, compared
with the cement. Thus, the volume of solids in the paste was
increased by replacing a definite weight of the cement with fly
ash. Moreover, the water demand of the mixture increased,
owing to the increase in the total surface area of the binder
(Mehta and Monteiro, 2006; Rana et al., 2016).
The mini slump values are presented in Table 9. As expected,
regardless of the WRA type, an increase in the mini slump
values of the paste mixtures was observed with an increase in
the use of admixture. However, the mini slump values of the
paste mixtures decreased or remained constant above a certain
admixture dosage, owing to the segregation. The chain length
variation of WRA at constant molecular weight did not sig-
nificantly affect the mini slump values. Conversely, an increase
in the mini slump values of the mixtures was observed with the
use of fly ash.
As can be seen from Table 9, the temperature of paste mixtures
decreased by 2–3°C with the increase in WRA content. This
was attributed to the set retarding effect of the WRAs, as well
to the inactivity of fly ash compared with that of the cement.
Time-dependent behaviour of mortar mixtures
The flow values of the mixtures were measured at time inter-
vals of 15 to 60 min to determine the effect of main and side
chain length changes of WRA with a constant molecular
weight on the time-dependent properties of mortar mixtures.
Fixed slump flow of mixture
In the first stage, the WRA requirement for a target flow was
determined. For this purpose, as seen in Figure 5, the flow of
the mixtures was measured by adding equal amounts of
WRAs in the range of 0.4–1 wt% of the binder to each
mixture. In this way, the amount of WRA providing 27 ± 2 cm
flow value was determined for each mixture. According to the

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Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

180 PC40k-1000-FA0 PC21k-2400-FA0 PC17k-3000-FA0

PC40k-1000-FA15 PC21k-2400-FA15 PC17k-3000-FA15
PC40k-1000-FA30 PC21k-2400-FA30 PC17k-3000-FA30
160
PC40k-1000-FA45 PC21k-2400-FA45 PC17k-3000-FA45
Marsh funnel flow time: s

140

120

100

80

60

40 Saturation point
20
1.00 1.25 1.50 1.75 2.00
WRA /binder: %

Figure 4. Marsh funnel flow times of the pastes with different dosages of admixtures

Table 9. Marsh funnel flow time, mini slump values and temperature of paste mixtures
Admixture dosage: % by weight of the binder

Property Mixture 0.75 1.00 1.25 1.50 1.75 2.00

Marsh funnel flow time: s PC40k-1000-FA0 No flow 79.74 62.16 53.34 51.78 50.41
PC21k-2400-FA0 No flow 74.34 55.75 45.14 44.01 42.65
PC17k-3000-FA0 No flow 98.88 76.47 64.70 62.97 61.22
PC40k-1000-FA15 No flow 107.14 68.32 57.14 56.60 57.70
PC21k-2400-FA15 No flow 102.21 64.64 49.75 48.00 47.56
PC17k-3000-FA15 No flow 124.16 81.89 61.60 61.12 61.00
PC40k-1000-FA30 No flow 133.76 79.40 72.38 71.90 71.18
PC21k-2400-FA30 No flow 129.98 71.37 66.65 65.66 64.32
PC17k-3000-FA30 No flow 140.65 92.76 78.86 77.42 76.90
PC40k-1000-FA45 No flow 148.84 102.08 88.26 88.84 87.32
PC21k-2400-FA45 No flow 138.97 98.90 82.76 80.45 80.00
PC17k-3000-FA45 No flow 154.54 113.13 100.09 94.67 94.56
Mini slump: mm PC40k-1000-FA0 8.3 12.3 15.5 17.5 17.0 17.5
PC21k-2400-FA0 10.8 15.5 17.3 18.3 17.5 18.0
PC17k-3000-FA0 9.0 14.5 16.5 17.5 16.8 17.3
PC40k-1000-FA15 10.3 13.8 15.5 16.0 17.0 16.5
PC21k-2400-FA15 12.5 16.3 17.0 18.5 17.5 16.5
PC17k-3000-FA15 12.0 15.3 16.0 16.5 17.0 16.5
PC40k-1000-FA30 12.3 14.5 16.0 16.3 16.5 16.8
PC21k-2400-FA30 14.5 16.3 16.8 16.8 16.5 16.8
PC17k-3000-FA30 13.0 15.5 16.3 16.5 15.8 17.3
PC40k-1000-FA45 13.5 15.3 15.5 16.0 17.5 15.8
PC21k-2400-FA45 14.8 16.0 16.5 16.5 16.3 16.5
PC17k-3000-FA45 13.5 15.5 15.8 17.0 16.8 15.8
Temperature: °C PC40k-1000-FA0 30.3 29.5 27.7 27.5 27.4 27.1
PC21k-2400-FA0 29.7 29.1 28.9 28.6 28.3 27.9
PC17k-3000-FA0 29.4 28.4 27.8 27.5 26.8 26.6
PC40k-1000-FA15 29.7 28.9 28.4 27.8 27.6 27.4
PC21k-2400-FA15 30.2 29.8 29.3 28.7 28.4 28.2
PC17k-3000-FA15 28.7 28.2 27.6 26.9 26.7 26.3
PC40k-1000-FA30 28.4 27.6 26.9 26.6 26.3 25.7
PC21k-2400-FA30 30.3 29.7 29.4 28.6 28.2 27.7
PC17k-3000-FA30 29.1 28.6 27.6 27.3 27.0 26.7
PC40k-1000-FA45 27.5 27.2 26.7 26.2 25.5 25.0
PC21k-2400-FA45 28.7 28.3 28.0 27.7 27.1 26.3
PC17k-3000-FA45 28.7 27.7 27.7 27.1 26.3 26.0

7
Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

31 31

29 ∗0.6% 29
∗0.56%

Flow: cm
Flow: cm

27 27
∗0.8% ∗0.7%
25 25
PC40k-1000-FA0 PC40k-1000-FA15
23 PC21k-2400-FA0 23 PC21k-2400-FA15
PC17k-3000-FA0 PC17k-3000-FA15

21 21
0.4 0.6 0.8 1.0 0.5 0.6 0.7 0.8
Admixture: % Admixture: %
(a) (b)
31 31

29 ∗0.5% 29
Flow: cm
Flow: cm

27 27

25 ∗0.6% 25
PC40k-1000-FA30 PC40k-1000-FA45
23 PC21k-2400-FA30 23 PC21k-2400-FA45
PC17k-3000-FA30 PC17k-3000-FA45
21 21
0.4 0.5 0.6 0.7 0.4 0.5 0.6 0.7
Admixture: % Admixture: %
(c) (d)

Figure 5. Admixture requirement to provide 27 ± 2 cm flow in mortar mixtures bearing: (a) 0% fly ash; (b) 15% fly ash; (c) 30% fly ash;
(d) 45% fly ash

Table 10. Time-dependent flow and V funnel flow times of mortar mixtures having a definite initial flow
Time-dependent flow: cm V funnel flow time: s

Mixture Admixture ratio: % 0 min 15 min 30 min 45 min 60 min 0 min 15 min

PC40k-1000-FA0 0.80 26.8 23.0 21.5 20.8 20.0 9.23 Blocked

PC21k-2400-FA0 0.60 26.8 21.8 20.3 19.3 18.3 6.73 Blocked
PC17k-3000-FA0 0.60 26.0 22.0 20.8 20.0 19.0 12.92 Blocked
PC40k-1000-FA15 0.70 26.3 22.0 21.3 20.5 20.0 11.68 Blocked
PC21k-2400-FA15 0.56 27.3 22.3 20.5 19.5 18.8 5.16 Blocked
PC17k-3000-FA15 0.56 25.5 21.5 20.0 19.5 18.8 20.37 Blocked
PC40k-1000-FA30 0.60 25.0 22.3 21.5 20.5 19.5 14.00 Blocked
PC21k-2400-FA30 0.50 28.3 22.5 21.3 20.3 19.5 8.96 Blocked
PC17k-3000-FA30 0.50 26.3 21.8 21.0 20.0 19.5 16.42 Blocked
PC40k-1000-FA45 0.50 25.5 23.0 21.8 21.0 20.3 Blocked Blocked
PC21k-2400-FA45 0.46 27.3 22.5 21.3 20.3 19.5 10.52 Blocked
PC17k-3000-FA45 0.46 25.3 23.0 21.8 21.0 20.3 Blocked Blocked

results, the desired flow value of the PC40k-1000-FA0 mixture
without fly ash was achieved by using 0.8 wt% of the binder.
The corresponding value was 0.6% for the PC21k-2400-FA0
and PC17k-3000-FA0 mixtures. These values were 0.7%,
0.56% and 0.56% for the PC40k-1000-FA15, PC21k-2400-
FA15 and PC17k-3000-FA15 mixtures, respectively, and 0.7%,
0.5% and 0.5% for the PC40k-1000-FA30, PC21k-2400-FA30
and PC17k-3000-FA30 mixtures, respectively. The ratios were
0.5, 0.46 and 0.46% for mixtures containing 45% ash. As can
be understood from the results, the admixture demand to
achieve target flow reduced with increasing fly ash substitution
level. This resulted from the dispersion of cement flocs by the
spherical and fine particles of fly ash, acting as ball bearings
among the cement grains, as well as from the easier adsorption
of WRA on the finer grains (Mardani-Aghabaglou et al.,
2017a, 2017b).
The flow loss of the mortar mixtures having an initial
27 ± 2 cm flow in a time period of 1 h are given in Table 10
and Figure 6. In terms of time-dependent flow performance,

8
Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

110 110
PC40k-1000-FA0 PC40k-1000-FA15
PC21k-2400-FA0 PC21k-2400-FA15
100 100
PC17k-3000-FA0 PC17k-3000-FA15
Relative flow: %

Relative flow: %
90 90

80 80

70 70

60 60
0 15 30 45 60 0 15 30 45 60
Time: min Time: min
(a) (b)

110 110 PC40k-1000-FA45

PC40k-1000-FA30
PC21k-2400-FA30 PC21k-2400-FA45
100 PC17k-3000-FA30 100 PC17k-3000-FA45
Relative flow: %
Relative flow: %

90 90

80 80

70 70

60 60
0 15 30 45 60 0 15 30 45 60
Time: min Time: min
(c) (d)

Figure 6. Time-dependent flow values of mixtures containing a definite amount of admixture and bearing: (a) 0% fly ash; (b) 15% fly
ash; (c) 30% fly ash; (d) 45% fly ash

Table 11. Time-dependent flow and V funnel test results (constant admixture amount)
Time-dependent flow: cm V funnel flow time: s

Mixture Admixture ratio: % 0 min 15 min 30 min 45 min 60 min 0 min 15 min

PC40k-1000-FA0 0.46 20.0 19.5 19.3 18.8 18.5 Blocked —

PC21k-2400-FA0 0.46 23.3 22.0 21.3 20.0 19.5 8.03 Blocked
PC17k-3000-FA0 0.46 21.0 20.5 20.5 20.0 19.3 Blocked —
PC40k-1000-FA15 0.46 21.5 21.0 20.5 19.8 19.0 Blocked —
PC21k-2400-FA15 0.46 24.8 23.8 22.5 21.0 20.0 8.66 Blocked
PC17k-3000-FA15 0.46 23.0 22.3 21.8 21.0 20.0 Blocked —
PC40k-1000-FA30 0.46 22.5 21.8 21.0 20.0 19.0 Blocked —
PC21k-2400-FA30 0.46 26.0 24.0 23.0 21.3 20.0 9.44 Blocked
PC17k-3000-FA30 0.46 24.8 24.0 22.8 21.5 20.5 Blocked —
PC40k-1000-FA45 0.46 25.5 23.0 21.8 21.0 20.3 Blocked —
PC21k-2400-FA45 0.46 27.3 22.5 21.3 20.3 19.5 10.52 Blocked
PC17k-3000-FA45 0.46 25.3 23.0 21.8 21.0 20.3 Blocked —

the most successful mixture was the PC40k-1000-FA0 mixture,
containing the admixture with the longest main chain and the
shortest side chain. After 60 min, the PC40k-1000-FA0
mixture showed 25% loss of flow, while the PC21k-2400-FA0
and PC17k-3000-FA0 mixtures showed 32% and 27% flow
loss, respectively. This trend was similar in all fly ash substi-
tuted mixtures. According to Felekoğlu and Sarikahya (2008),
the faster the admixture adsorption on the cement grains, the
higher the initial flow performance of the mixture. However,
high adsorption of the admixture affects the flow retention of
the mixture negatively. In other words, the workability reten-
tion is directly proportional to the amount of free admixture in
the mortar mixture (Surico, 2008). It is well known that
admixture chains can be intertwined with each other if the

9
Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

Fixed flow Fixed admixture content

100

80
Flow: cm

60

40

20

0
15

15

45

45

45
0

15

30

30

30
FA

FA

FA

FA

FA

FA

FA

FA
FA

FA

FA

FA
0-

0-

0-

0-

0-

0-

0-

0-
0-

0-

0-

0-
00

40

00

00

40

00

40

00
00

00

40

00
1

3
k-

k-

k-

3
k-

k-

k-

k-

k-
k-

k-

k-

k-
40

21

17

40

21

40

21

17
17

40

21

17
PC

PC

PC

PC

PC

PC

PC

PC
PC

PC

PC

PC
Figure 7. Relative flow values of mortar mixtures having either a constant flow or a constant admixture content at the end of 60 min

main or side chains are too long (Kong et al., 2016; Qiu et al.,
2011; Zingg et al., 2009). As a result, there is a special relation-
ship between the main chains, side chains and anionic mono-
mers of the admixtures in terms of adsorption and dispersion.
While the admixture adsorbed onto the cement provides fluid-
ity in the mixture, the free admixture in the solution controls
the workability retention of the cementitious system.
Therefore, it may be claimed that fluidity performance and
workability retention are inversely interrelated. Among the
admixtures used in this study, PC21k-2400 showed the best
performance in terms of initial flow in plain and fly ash mix-
tures but the worse performance in terms of flow retention.
Test results of time-dependent V funnel flow of the mortars are
shown in Table 10. Since the mixtures did not flow through the
V funnel 15 min after casting, only the initial flow times could
be measured. The V funnel flow performance of the mortars
was very similar to the Marsh funnel flow performance of their
counterparts. Among the plain mixtures, the PC21k-2400-FA0
mixture showed the fastest flow from the V funnel, whereas the
slowest flow time was recorded for the PC17k-3000-FA0
mixture. Irrespective of the binder type, flow performances of
the mixtures containing admixtures with short main chains and
long side chains were negatively affected, owing to insufficient
electrostatic and steric effects. Partial replacement of a definite
weight of cement with fly ash increased the volume of solids in
the mixture, resulting in an increase in the viscosity and a conse-
quent reduction in the flow of the mix.
added to the 45% fly ash mixtures without any segregation.
The time-dependent flow values of the mixtures with fixed
admixture amount are given in Table 11. The PC30k-1000
admixture showed the best performance in terms of mortar
flow retention. The relative flow values of the mortar mixtures
having either a constant flow value or a fixed admixture
content at the end of 60 min are shown in Figure 7. It was
revealed that consistency loss (after 60 min) was less in the
mixtures containing less WRA. However, no meaningful
relationship was found between admixture dosage and loss of
mortar consistency. This fact is attributed to the loss of effec-
tiveness of the WRA with elapsing time. As is already known,
if the desired flow value is provided by adding water, the
mixture can maintain its flow for a longer time compared with
the situation where the flow is achieved by adding a WRA.
According to the results of the flow test, the initial flow of the
mixtures increased with the use of fly ash, regardless of the
main and side chain lengths of the admixtures. This effect was
more pronounced with the increase in fly ash substitution level.
Meanwhile, irrespective of WRA type, 1 h flow loss of the
mixtures increased with increasing fly ash inclusion level. The
fly ash used in this study had a higher fineness and a lower
specific gravity than those of the cement. Therefore, fly ash
substitution increased both the volume of binder and the
surface area/volume ratio of binder particles in the mix. As a
result, the water requirement for a given consistency and the
loss of consistency with elapsing time increased with increasing
substitution level.

Fixed amount of admixture
In the mortar mixtures having a definite flow, the admixture
content was variable. To provide a clear idea of the effect of
the length of the admixture chains on the behaviour of the
cementitious system, mortar mixtures containing a fixed
amount of admixture (0.46 wt% of binder) were prepared.
This admixture dosage was the maximum dosage that could be
Regardless of the admixture chain lengths and fly ash substi-
tution level, a strong linear relationship between the flow
values and the mini slump values was found (Figure 8).
The V funnel flow time values of the mixtures having a fixed
admixture content are given in Table 11. The mixture contain-
ing the PC21k-2400 admixture initially flowed through the V

10
Magazine of Concrete Research Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar

funnel while the mixtures containing the PC40k-1000 and to be 8, 18 and 31% longer, respectively, compared with those
PC17k-3000 admixtures did not flow from the funnel. This of the PC21k-2400-FA0 mixture.
was the case in all of the mortars 15 min after their prep-
aration. The V funnel flow times of PC21k-2400-FA15,
PC21k-2400-FA30 and PC21k-2400-FA45 mixtures were found Compressive strength
The compressive strength values of 1, 3, 7, 28 and 90 day
mortar specimens are given in Table 12. As can be seen from
30 Table 12, the early- and late-age compressive strengths of the
y = 1.0272x + 11.381 mortar mixtures were not severely affected by the change in
27
R2 = 0.95 main and side chain lengths of the admixture, regardless of fly
Flow: cm

24 ash substitution level.

21 Conversely, as expected, the fly ash substitution level adversely

18 affected the 1, 3 and 7 day compressive strength of mortar
mixtures. This negative effect increased even more with the
15 increase in fly ash substitution level. However, as a result of
4 6 8 10 12 14 16
the development of the pozzolanic reaction with elapsing time,
Mini slump: cm the strength difference between the mixtures decreased. Fly ash
Figure 8. Relationship between mini slump and flow values substitution up to 30% improved the compressive strength of
mortar mixtures beyond 28 days, while 45% fly ash substi-
tution reduced the compressive strength (compared with that
of the control mix) at all ages, even 90 days.
Table 12. Compressive strength of mortar mixtures
Compressive strength: MPa
Water absorption capacity
Mixture 1 day 3 days 7 days 28 days 90 days
The 28 and 90 day water absorption ratios of mortar mixtures,
PC40k-1000-FA0 7.5 26.8 36.9 43.6 49.4 shown in Figure 9, varied in the range 6.2–8.3%. The changes
PC21k-2400-FA0 7.2 26.8 33.7 38.8 46.7 in the length of WRA main and side chains at constant mol-
PC17k-3000-FA0 9.5 28.3 36.1 42.7 49.2 ecular weight did not significantly affect the water absorption
PC40k-1000-FA15 6.7 25.7 36.5 43.9 51.0
of the mortar mixtures. Fly ash inclusion reduced water
PC21k-2400-FA15 6.4 23.8 32.2 40.1 48.2
PC17k-3000-FA15 8.8 26.6 35.9 46.8 53.8 absorption, particularly in 90 day specimens. This positive
PC40k-1000-FA30 4.1 21.7 25.6 41.2 52.0 effect arises from the physical pore-filling effect of fine fly ash
PC21k-2400-FA30 5.1 21.4 26.7 41.4 50.8 particles, as well as the chemical pozzolanic reaction of the fly
PC17k-3000-FA30 4.8 23.2 29.7 41.5 57.7 ash, resulting in a strong and uniform matrix and interfacial
PC40k-1000-FA45 1.8 14.1 20.3 32.4 39.5
transition zone on reduction of capillary porosity of the
PC21k-2400-FA45 3.9 15.7 21.2 32.5 44.2
PC17k-3000-FA45 3.2 15.3 21.9 32.6 42.8 mixture (Mardani-Aghabaglou et al., 2014; Mehta and
Monteiro, 2006).

10
28 days 90 days
Water absorption rate: %

0
5

45
0

0
A1

A1

A4

A4
FA

FA

FA

A1

A3

A3

A3

FA
-

-F

-F

-F

-F
-F

-F

-F

-F
00

00

00

-
00

00

00

00

00
00

00

00

00
10

24

30

10

24

10

24

30
0

0
k-

k-

k-

-3

-1

-2

-3
k-

k-

k-

k-

k-
40

21

17

k
40

21

40

21

17
17

40

21

17
PC

PC

PC

PC

PC

PC

PC

PC
PC

PC

PC

PC

Figure 9. Water absorption rates of mortars

11
Magazine of Concrete Research
Conclusion
The findings of the research study can be summarised as
follows.
& The FTIR spectra curves of admixtures with different
chain lengths at constant molecular weight are close to
each other.
& The TOC analysis results reveal that the admixture
with 17k of main chain and the longest side chains
showed the highest adsorption on cement grains, while
the adsorption of the admixture with 21k of main
chain length and 2400 g/mol of side chain length was
the lowest.
& Decreasing the lengths of the side and main chains of the
WRA decreased its electrostatic and steric effects,
respectively. Moreover, the flowability of the mixtures was
negatively affected with increasing length of the main and
side chains of the polymers. The admixture with medium
main chain length (21k) and medium side chain length
(2400 g/mol molecular weight) showed the best Marsh
funnel and V funnel flow time performance.
& The admixtures with long main chain or long side chains
exhibited better flow retention of the mortars. Regardless
of the properties of the WRA, flow performances were
generally adversely affected by adding fly ash to the paste
mixtures. This adverse effect was more pronounced with an
increase in ash substitution level. However, the WRA
requirement for a given flow reduced with the use of fly ash
in mortar mixtures.
& The change in length of the main and side chains of the
WRA caused similar effects on the fresh properties of plain
(no fly ash) and fly ash cementitious systems.
& The change in length of the main and side chains of the
WRA (with a fixed molecular weight) showed no
considerable effect on the early- and late-age compressive
strengths and water absorption capacities of the mortar
mixtures. Regardless of the WRA type, fly ash inclusion
reduced the early strength of the mixtures but improved
their late strength and impermeability. The optimum fly
ash utilisation ratio in terms of mortar strength was found
to be 30%.
Acknowledgements
The authors appreciate contributions of the Scientific and
Technological Research Council of Turkey (TUBITAK) and
Bursa Uludag University Science and Technology Centre
(BAP) (grant numbers 219M425, AYP (MH)-2016/16, DDP
(MH)-2018/9, DDP(MH)-2019/15). In addition, the first
author acknowledges the scholarship provided by TUBITAK
(grant number 217M408) during his PhD study. The authors
also thank authorities from the Polisan Construction
Chemicals Company and Bursa-Beton Ready Mixed Concrete
for their kind assistance in providing the cement, aggregate
and WRAs, as well as determining their properties.
12
Multi-effect of superplasticisers main and
side-chain length on cementitious
systems with fly ash
Özen, Altun, Mardani-Aghabaglou and
Ramyar
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