Construction and Building Materials 147 (2017) 669–676

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Construction and Building Materials

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

Super absorbent polymers (SAPs) as physical air entrainment in cement

mortars
Siamak Riyazi a,⇑, John T. Kevern a, Matt Mulheron b
a
Department of Civil Engineering, University of Missouri-Kansas City, Kansas City, MO, United States
b
Talon Concrete and Aggregates, Kansas City, MO, United States

h i g h l i g h t s

 Size and number of voids are increased with increasing SAP dosage.
 Absorption decreased with increasing SAP dosage.
 The SAP enhanced concrete has sufficient air void system.

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

Article history: Super absorbent polymers (SAPs) are novel multipurpose materials in concrete technology. This study
Received 17 February 2017 investigated the potential for using SAPs as a mechanism for physical air entrainment. Mixtures were
Received in revised form 26 April 2017 produced using various quantities of either dry or pre-saturated SAP along with a conventionally air-
Accepted 1 May 2017
entrained control. One additional mixture used lightweight fine aggregate as a mechanism for physical
air entrainment. The quality of the air void system was investigated using a high resolution flatbed scan-
ning and image analysis. It was found that one-dimensional water absorption decreased with increased
Keywords:
SAP dosage suggesting that SAP would not increase degree of saturation during freezing and thawing.
Super absorbent polymer (SAP)
Image analysis
Various dosage rates and conditions of SAP were able to produce adequate air void systems with satisfac-
Absorption tory size and distribution as compared to conventional air entraining agents.
Void distribution Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction consistent dosage rates of AEAs difficult. A promising method to

Concrete is the most handled man-made material on earth with
more than 2.5 tons produced per person per year [1]. Freeze and
thaw deterioration is one of the primary concerns for concrete
durability in cold climates. Concrete is air-entrained to improve
durability and ultimately service life. Traditionally air voids are
produced in concrete using chemical air-entraining agents (AEAs).
These surfactants stabilize the air bubbles created during concrete
mixing and prevent small bubbles from coalescing and escaping
[2]. Air content in concrete containing AEAs can be highly variable
and is impacted by variables such as temperature, haul time and
agitation, pumping and internal vibration. Chemical incompatibil-
ities with superplasticizers, loss of air during consolidation and
coalescence of air bubbles in fresh concrete are examples of other
technical issues in using AEAs [3]. Additionally, variability in fly
ash sources, quality, and impurities such as unburnt carbon make
⇑ Corresponding author.
E-mail address: srvgd@mail.umkc.edu (S. Riyazi).
achieve stable air voids in concrete is physical air entrainment
where predefined size and spacing of air voids are added to fresh
concrete which avoids the previously mentioned issues with sur-
factant AEAs. In 1978, Litvan and Sereda conducted a feasibility
study using crushed brick and diatomaceous earth as porous mate-
rials to create a desired physical air voids system [4]. They found
using materials with porous media can offset the negative effects
of conventional AEA on strength in concrete. In addition, they
observed the porous material significantly decreased the freeze-
thaw deterioration. In 2001, Jensen and Hansen conduct a pioneer-
ing research in the first phase investigated the principles and the-
oretical background of water entrainment in concrete [5]. In 2002,
the second phase of their investigation reported that SAPs can
improve the concrete performance against autogenous shrinkage
and cracking during restrained hardening [6].
SAPs were first developed in 1980s and are mainly used in con-
venience products, food packaging, and sanitary and medical
industry e.g. care articles or smart pills [7,8]. SAPs have the ability
to absorb water, expand, and retain the liquid in the space between

http://dx.doi.org/10.1016/j.conbuildmat.2017.05.001
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
670 S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676
the polymer chains and crosslinks without being dissolved into
solution [9,10]. Different amounts of liquid absorption have been
reported for various types of SAPs and generally ranges from 500
times [9] to over 1500 times absorption by weight [7]. Common
SAPs are covalently hydrophilic networks of cross-linked poly
acrylic acids which consist of long chains of linear polymers inter-
connected at several points [9]. Osmotic pressure is the driving
force of liquid into the polymer structure which causes swelling
and creates a hydrogel [9,11].
There are two major methods to synthesize the polymers
including bulk polymerization and inverse suspension polymeriza-
tion. In the first method, blocks of polymer are crushed into smaller
irregular shaped particles with predefined size distribution. Second
method uses inverse suspension polymerization technique. Unlike
the first method, particle shape in second method is spherical [12].
Depending on which kind of polymers is used in concrete mixture,
resulting air voids will either have irregular or near spherical
shape. The swelling capacity of the polymer in concrete mixture
should be taken into consideration in choosing the right type of
SAP since this factor is decreased in high saline and high pH envi-
ronment [13]. It is well discussed that the amount of absorbed liq-
uid in polymer is dependent on the fluid chemistry in vicinity of
SAP [10,13]. Generally, the absorption capacity is decreased in liq-
uids containing ion such as Ca2+ and Al3+ [7]. The highest amount of
absorption for most SAPs occurs in distilled or deionized water
[14]. Absorbed water in SAP acts as a reservoir of free water and
has made these polymers promising materials to used with cemen-
titious materials in concrete for reducing the autogenous shrinkage
via internal curing [5,6,12,14–22] and increasing the durability
against freeze and thaw deterioration [23,24]. Improvement of
autogenous healing [25,26], improving tensile creep [27], and
changing the rheology of the fresh material [17,23,28,29] are other
important characteristics of SAP enhanced concrete.
According to the literature, internal curing effect of SAPs is
almost completed in first couple of days after mixing due to the
SAP pore solution extrication in the initial days of hydration [6].
Mönnig investigated the desorption kinetics of SAPs and shown
water transport from SAP particle almost completed in initial hours
of hydration [30]. Nestle et al. observed after 24 h of hydration no
water remaining in the SAP particle in cement paste [31]. In the lit-
erature, researchers have primarily focused on general characteris-
tics of SAP-enhanced concrete without considering this material as
an alternative method to ordinary air entrainment using AEAs [7–
10,23,24]. Air void system produced by SAPs is an area which
requires research to clarify how SAP incorporation affects hard-
ened properties of concrete to improve concrete durability against
freeze and thaw deterioration. The objective of this study was to
investigate the development of the air system in concrete
enhanced with dry and pre saturated SAP. Compressive strength
and water absorption tests were carried out as a comprehensive
experimental evaluation. The hardened air void system was inves-
tigated using high resolution flatbed scanning and imageJ analysis.
The combination of all characteristics has given a general overview
of the effects of SAPs on durability and other properties of concern
and indicate that SAPs can produce an air void system comparable
to conventional AEAs.
2. Experimental program
2.1. Materials
ASTM C150 Type I Portland cement was used in this study [32].
The specific gravity and Blaine fineness of cement were 3.15 and
373 m2/kg, respectively. Table 1 lists the chemical composition of
cement. Standard concrete washed river sand was used as fine
Table 1
Chemical composition of cement.
Chemical properties Cement (%)
CaO 63.48
SiO2 20.49
Al2O3 4.26
Fe2O3 3.14
MgO 2.11
SO3 2.9
K2O 0.47
Na2O 0.18
Ignition loss 2.2
Remaining insoluble (RI) 0.2
Alkaline equivalents (AE) 0.49
aggregate with specific gravity, fineness modulus, and water
absorption of 2.51, 2.79, and 2.6%, respectively. The gradation of
fine aggregate conformed to ASTM C33 [33].
A commercially available polymerized polyacrylate was used as
SAP with specific gravity, pH values and cation exchange capacity
of 1.1, 8.1 and 4.6 meq/g respectively. Specifically the SAP material
was bulk-polymerized crushed crystalline partial sodium salt of
cross-linked polypromancic acid with irregular shape. Since high
ionic strength solutions reduce the absorption capacity of certain
SAPs [12,34–39], in this study deionized (DI) water was used to
pre-saturate the SAP with the absorption capacity of 2000 times
of weight of dry polymer.
2.2. Mixture proportions, sample preparation, and testing
The SAP mixtures were designed with w/cm of 0.48. SAP types
(noted as SAP for dry polymer and PSAP for pre-saturated) were
incorporated at different dosages of 0.06, 0.12, 0.25, 0.5, 1 and 2
percent by weight of cement. Two control mixtures were produced
with/out air-entraining admixture. The AEA was a commercially-
available vinsol resin. The total amount of water was not changed
between the mixtures containing the dry or presaturated SAPs. The
mortar had a ratio of 2.5:1 dry river sand to cement by weight. The
mixture proportions are given in Table 2 with oven-dry weights of
fine aggregate. One additional mixture was used which contained
prewetted lightweight fine aggregate (LW) which volumetrically
replaced the standard sand but dosed to produce 6% total air
within the mortar. The lightweight aggregate was expanded shale
with a wetted surface dry (WSD) condition of 16% tested according
to ASTM C1761 [40].
All samples were mixed according to ASTM C305 [41]. The SAP
was incorporated either dry or pre-saturated prior to incorporation
in the mortar mixtures. The prehydration was performed by plac-
ing the desired dosage of SAP in the entire quantity of mixing
water 12 h before sample preparation. For concrete specimens con-
taining dry SAP, dry polymer was added to mixtures during the
mixing procedure. Cubes were cured in a moist room meeting
ASTM C511 requirements until testing [42]. Compressive strength
was tested at 7 days according to ASTM C109 [43]. All strength data
represents an average of three specimens. Rate of absorption of
water was tested according to ASTM C1585 and data also repre-
sents an average of three specimens [44].
Prior to air system image analysis cubes were removed from
moist curing and dried at 50% relative humidity and 23 °C for
14 days. To analyze air voids in the mortar cubes each were sawn
in half. Then all the samples were cleaned in ultrasonic bath with
hot, soapy water. All samples were progressively ground and wet
polished through 9 mm grit on a 180 rpm lapping wheel. After pol-
ishing samples were again cleaned in the ultrasonic bath. Polished
surfaces were colored black with a wide felt-tip pen in two perpen-
dicular sets. Samples were then coated with a white mixture of
 S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676 671

Table 2
SAP concrete mix proportions.

Mixture notation w/cm Cement (kg/m3) Water (kg/m3) Fine aggregate (kg/m3) SAP (% of cement) AEA (% of cement)
C1 0.48 571 281 1428 – –
C2 0.48 571 281 1428 – 0.07
SAP1 0.48 571 281 1428 0.06 –
SAP2 0.48 571 281 1428 0.12 –
SAP4 0.48 571 281 1428 0.25 –
SAP8 0.48 571 281 1428 0.50 –
SAP16 0.48 571 281 1428 1.00 –
SAP32 0.48 571 281 1428 2.00 –
PSAP1 0.48 571 281 1428 0.06 –
PSAP2 0.48 571 281 1428 0.12 –
PSAP4 0.48 571 281 1428 0.25 –
PSAP8 0.48 571 281 1428 0.50 –
PSAP16 0.48 571 281 1428 1.00 –
PSAP32 0.48 571 281 1428 2.00 –
LW 0.48 571 281 980/450WSD – –

titanium dioxide and petroleum jelly. Sufficient force was used to no differences in compressive strength between pre saturated
ensure all the voids were filled with white paste. Using the edge SAP and dry SAP except for samples with SAP dosage of 0.5 and 1
of a blade, the excess paste was wiped off from the surface. The percent of cement weight (SAP8 and SAP16).
specimens were scanned using high resolution flatbed scanner Results of the air void analysis is shown in Table 3. The data
and analyzed with ImageJ software [45]. shown represents an average of four scans each rotated 90° for
all three samples. The coefficient of variation (COV) was generally
3. Test results and discussion low and indicates good precision for the test method. For durability
against freezing and thawing the voids should be small and dis-
Fig. 1 shows the compressive strength results for the control persed evenly throughout the concrete paste. Specific surface area
samples along with the samples containing LW, dry and prehy- (the surface area of the average void divided by the volume of the
drated SAPs. As expected the mixture with AEA had significantly average void) represents the bubble size and spacing factor repre-
lower compressive strength than the mixture without AEA. The senting the distribution. As expected the mixture without air-
mixture containing LW, also without AEA, produce significantly entrainment (C1) had the lowest total air content of 1.0% with
higher compressive strength than either. Although the w/cm for the air-entrained mixture (C2) having 6.2% total air. The mixture
these mixtures was 0.48, presumably the increase in strength containing LW had 5.2% total air and similar specific surface area
was a result of internal curing and any pozzolanic contribution of to C2, however the spacing factor was an order of magnitude
the expanded shale. Concrete samples containing dry polymer higher than the other specimens. This is because all of the voids
did not show any distinct trends. As it is shown in Fig. 1, the spec- are wholly contained within the aggregates which results in
imen with SAP dosage of 0.5 percent of cement weight (SAP8) has unair-entrained paste surrounding the LW pieces. For both the
the highest 7-day compressive strength among all other samples dry (SAP) and prehydrated (PSAP) mixtures total air content
containing dry polymer. SAP8 has also higher compressive strength increased with increasing SAP dosage ranging from 2.8% (PSAP1)
comparing to control sample with no AEA (C1). Except SAP32, all to 14.7% (SAP32). Generally, the air system produced by the SAP
other samples have showed higher compressive strength compar- resembled that of the surfactant AEA. Both 0.5% dosage (SAP8
ing to control specimen with AEA (C2). For the prehydrated mix- and PSAP8) conditions produced the air system characteristics
tures there was a decrease in strength with increased dosage most closely matching the air-entrained mixture (C2).
beyond 0.125% (PSAP2). The highest two dosages of 1% and 2% by Figs. 2–4 are binary images of concrete specimens prepared for
weight of cement did result in a decrease in strength. Compressive air void analysis. Black areas are air voids and white background is
strength data sets were compared using analysis of variance the concrete paste/aggregates. In Fig. 2 there is a distinct visual dif-
(ANOVA) with a = 0.05. At comparable dosage rates there were ferent between the unair-entrained mixture (C1) and the air-

50

45
7-Day Compressive Strength(MPa)

40

35

30

25

20

15

10
PSAP16

PSAP32
PSAP1

PSAP2

PSAP4

PSAP8
SAP16

SAP32
SAP1

SAP2

SAP4

SAP8

5
LW
C1

C2

Fig. 1. 7-Day compressive strength of concrete cubes having different dosage of dry/prehydrated SAPs and concrete with lightweight aggregate.
672 S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676

Table 3
Bubble counter data.

Sample Specific Surface Spacing Factor (mm) Air  1 mm Total Air

1
(mm ) COV (%) (mm) COV (%) (%) COV (%) (%) COV (%)
C1 73.46 12.6 0.054 16.4 0.7 4.4 1.0 5.6
C2 33.42 8.1 0.043 12.9 4.4 2.7 6.1 1.3
LW 42.33 8.4 0.308 4.6 4.3 1.5 5.2 0.9
SAP1 27.15 5.4 0.097 2.6 3.7 2.6 5.0 1.2
SAP2 20.19 9.6 0.100 10.8 3.7 1.5 5.4 0.4
SAP4 28.57 6.1 0.081 10.9 3.9 1.7 5.5 2.0
SAP8 41.15 4.2 0.031 11.1 3.1 1.9 6.2 1.4
SAP16 33.34 10.0 0.039 10.2 3.4 1.5 7.8 1.9
SAP32 19.63 6.5 0.035 8.8 3.4 2.2 14.7 2.8
PSAP1 32.45 13.0 0.120 2.1 2.0 3.3 2.8 2.5
PSAP2 40.43 3.8 0.076 15.9 3.1 2.9 3.9 1.8
PSAP4 37.17 11.2 0.072 11.6 3.0 4.0 4.0 4.8
PSAP8 36.87 6.3 0.027 3.5 5.0 2.1 6.0 1.6
PSAP16 37.10 3.5 0.025 4.3 5.2 2.9 6.4 3.2
PSAP32 38.42 2.2 0.027 4.1 4.3 3.5 6.3 4.1

Fig. 2. Binary image of controls and lightweight aggregates specimens.

entrained control C2. The mixture containing LW possess the nat-
ural round air voids of C1 but also the much finer voids contained
within the lightweight aggregate. Fig. 3 shows the progression of
air void development with increased dry SAP dosage. At lower
dosages the voids were much more round compared with the high
dosages where incomplete dispersion and clumping were
observed. Fig. 4 shows the sample image progression for the mix-
tures containing the prehydrated SAPs. Visually it appeared pre-
hydrating produced better dispersion, less clumping, and more
rounded voids. Consequently, air distribution was mapped for a
more quantitative analysis.
Fig. 5 is the cumulative distribution of air voids in concrete mix-
tures containing the dry SAP. The vertical line corresponds to air void
size of 1 mm which is assumed as the border between entrained air
voids and entrapped air voids based on ASTM C 457 [46]. The mix-
ture containing the lightweight aggregate (LW) had the finest grada-
tion of bubbles followed by the unair-entrained mixture (C1) and the
air-entrained mixture (C2). Mixtures SAP1, SAP2, SAP4, and SAP 8
had similar, yet much coarser air system. The highest two dosages
for the dry SAP (SAP 16 and SAP32) had the coarsest air system which
was evident from the clumping observed in Fig. 3. Fig. 6 shows the
same air bubble gradation, but for the pre-hydrated SAP mixtures.
At the very small sizes (<0.1 mm), generally the PSAP air system
was coarser than the air-entrained control (C2). Other than the
entrapped portion (>1 mm) of the highest dosage (PSAP32) the air
system characteristics were similar between the PSAP mixtures
and the air-entrained control (C2).
Initially one point of concern for the incorporation of SAP in
concrete mixtures is the potential for rehydration in the matrix,
increasing the exposure condition and reducing durability. Conse-
quently, one-dimensional absorption was performed according to
ASTM C1585. Fig. 7 compares absorption of control samples
with/without AEA and the mixture with lightweight aggregate.
The unair-entrained mixture (C1) had the highest absorption fol-
lowed by the lightweight aggregate mixture (LW) and the air-
entrained mixture (C2). Since entrained air bubbles do not saturate
under normal conditions, the reduction in absorption with air-
entrainment is due to the dilution of the absorbing hydrated paste
with the unabsorbing voids. The reduction in absorption for LW is
most likely a combination of dilution, densification of the hydrated
paste from internal curing, and densification of the hydrated paste
from any pozzolanic reaction. Fig. 8 shows the absorption of the
mixtures containing dry SAP. All mixtures had less absorption than
the air-entrained control with absorption decreasing with increas-
ing SAP dosage. Fig. 9 shows absorption for the mixtures contain-
ing prehydrated SAP and following the same trend as the dry SAP
mixtures. A comparison of all mixtures is shown in Fig. 10. In all
cases except the 1% dosage, all prehydrated variants had lower
absorption than the dry version at equal dosage rate. Since SAPs
do provide internal curing benefit the decrease is most likely a
combination of dilution and internal curing benefit. The observa-
tion of lower permeability is consistent with a densification of
the cementitious matrix through internal curing reported in the lit-
erature [24,26,47,48]. All SAP combinations had less absorption
S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676 673

Fig. 3. Binary image of specimens containing dry SAP.

Fig. 4. Binary image of specimens containing prewetted SAP.

674 S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676

C1 C2 LW C2 SAP1 SAP2
SAP1 SAP2 SAP4 SAP4 SAP8 SAP16
SAP8 SAP16 SAP32 SAP32
100 5
90 4.5
4
Accumulative total air (%)

80

Absorption (mm)
70 3.5
3
60
2.5
50 2
40 1.5
30 1
20 0.5
10 0
0 500 1000
0 Sqrt (time, seconds)
0.5-1
1.5-2
2.5-3
3.5-4
4.5-5
5.5-6
6.5-7
0.02-0.03
0.04-0.05
0.06-0.07
0.08-0.09

0.14-0.16

0.22-0.24
0.26-0.28
0-0.01

0.1-0.12

0.3-0.35
0.18-0.2

0.4-0.45

Fig. 8. Absorption of control mixtures and concrete containing dry SAP.

Size (mm)

Fig. 5. Cumulative distribution of air voids in concrete mixtures containing dry SAP.

C2 PSAP1 PSAP2
C1 C2 LW PSAP4 PSAP8 PSAP16
PSAP1 PSAP2 PSAP4 PSAP32
PSAP8 PSAP16 PSAP32 5
100 4.5
90 4
Absorption (mm)

3.5
Accumulative total air (%)

80
70 3
60 2.5
2
50
1.5
40
1
30 0.5
20 0
10 0 500 1000
0 Sqrt (time, seconds)
0.02-0.03
0.04-0.05
0.06-0.07
0.08-0.09

0.14-0.16

0.22-0.24
0.26-0.28
0-0.01

0.18-0.2

0.5-1
1.5-2
2.5-3
3.5-4
4.5-5
5.5-6
6.5-7
0.1-0.12

0.3-0.35
0.4-0.45

Fig. 9. Absorption of control mixtures and concrete containing pre-saturated SAP.

Size (mm)

Fig. 6. Cumulative distribution of air voids in concrete mixtures containing pre-

wetted SAP. 7

6
Absorption after 8 days (mm)

C1 C2 LWA
5
7
6
4
5
Absorption (mm)

4 3
3
2 2

1
PSAP16

PSAP32

1
PSAP2

PSAP8

SAP16

SAP32
SAP2

SAP8

0
LW

0 500 1000
C1

C2

Sqrt (time, seconds) 0

Fig. 7. Absorption of control mixtures and lightweight mix. Fig. 10. Absorption at 8 days.
 S. Riyazi et al. / Construction and Building Materials 147 (2017) 669–676
than any of the control specimens indicating the potential for bet-
ter freeze-thaw durability.
4. Conclusion
Super absorbent polymers (SAPs) represent a novel water
absorbing material that have shown benefit to concrete through
internal curing. Many factors cause variable air entraining when
using surfactants including but not limited to temperature, mixing
time, fly ash, pumping, and internal vibration. This study investi-
gated the potential of using SAP as a mechanism for mechanical
air-entrainment. Mixture variants were produced with dry SAP
and prehydrated SAP incorporated into the mixture. Compressive
strength, air system properties, and absorption were measured.
From this study the following conclusions can be drawn:
 Compressive strength generally decreased with increased SAP
dosage. All dosages 0.5% by weight of cement or less produced
higher compressive strength than the air-entrained control
samples. The highest compressive strength in the study was
achieved by the mixture which included prewetted lightweight
fine aggregate dosed to produce 6% total mixture voids.
 Higher dosages of both pre-hydrated SAP and dry SAP produced
more voids with larger bubble size and lower specific surface
area.
 The voids produced by dry SAP were more angular than the
voids produced by the prehydrated SAP and more similar to
the shape of voids produced by the conventional air-
entraining agent.
 The distribution of air void sizes was much coarser for the SAP
added to the mix dry, while the distribution of the prehydrated
SAP voids was similar to the conventional air-entraining agent.
The finest void system was produced by the lightweight aggre-
gate, however the spacing factor was significantly higher due to
the voids only occurring in the included fine aggregate.
 Absorption decreased with the inclusion of SAP linearly with
dosage rate as compared with the air-entrained control mix-
ture. At equal dosages the prehydrated SAP had less absorption
than the similar mixture prepared with dry SAP.
 The SAP was able to produce an adequate air void system with
satisfactory size and distribution similar to the control mixture
containing standard air entrainment admixture.
Acknowledgments
The authors acknowledge with gratitude the financial support
of the University of Missouri-Kansas City; School of Graduate
Studies.
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