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Abstract: The use of superabsorbent polymers (SAP) is one internal curing method being adopted for
the mitigation of autogenous shrinkage in concrete especially high strength/performance concrete
(HSC/HPC). SAP absorbs water and releases the water internally when cement hydrates. It however
leaves micro voids in this process and this can negatively influence the mechanical properties of
concrete. This paper reports on three dimensional (3D) volume analysis of the influence of SAP
content and curing age on air voids distribution in HPC. Four HPC mixtures with different binder
constituents and water/binder (W/B) ratios: M1 and M1D (0.2), M2 (0.25) and M3 (0.3) were tested with
two grain sizes of SAP ( 300 m with product label FLOSET CS 27 and 600 m, labelled FLOSET
CC 27). The SAP contents were also varied (0%; 0.2%; 0.3%; and 0.4%) by weight of binder.
Concrete cylinders (50 mm in diameter and 100 mm high) were cast and cured in water for different
ages (28, 56 and 90 days) before the dry hardened HPC was subjected to X-ray computed
tomography (CT) scanning for determination of the air void distribution. The 3D X-ray images were
then examined and analysed using Avizo Fire image analysis software version 8.0 to filter and
classify the individual voids for determination of the sizes, distribution and volume analysis of void
created by SAP in the HPC with the respective influence of binder type, water/binder ratio and curing
age assessed. The CT scanning was also used to affirm the grain sizes and distribution of the dry
SAP particles.
Keywords: Computed tomography (CT) scanning, 3D - void analysis, high - performance concrete,
air void distribution, superabsorbent polymers (SAP), SAP content, binder type, curing age.
INTRODUCTION
Concrete is a versatile material for construction works but it however requires adequate curing for
effective strength development, durability and mechanical characteristics. In conventional concrete,
the curing methods of immersion in water, sprinkling and others as provided for in the codes of
concrete practice [1, 2] suffice for prevention of moisture loss from the concrete surface. Highperformance concrete (HPC) on the other hand, is defined ACI as concrete meeting special
combinations of performance and uniformity requirements that cannot always be achieved routinely
using conventional constituents and normal mixing, placing, and curing practice [3]. HPCs are
typically of low water/binder (W/B) ratios that may not supply enough water to hydrate all of the
cement. The reduction in permeability of HPC even within the first 2 to 3 days makes exterior water
curing inadequate in supplying hydration to the cement as the hydration products fill in and disconnect
the capillary pore network [4, 5].
The growing trend in the utilisation of high-performance and ultra-high-performance concrete (HPC
and UHPC) in the construction industry and the susceptibility of this concrete types to self-desiccation
and autogenous shrinkage thereby necessitated research into materials for internal curing of concrete
(IC-agents) such as saturated lightweight aggregates (LWA) and Superabsorbent Polymers (SAP)
amongst others [6, 7, 8].
The use of SAP as IC-agent has been adjudged to be effective for the mitigation of autogenous
shrinkage in concrete especially HSC/HPC via its absorption and desorption of water internally as the
cement hydrates. It however leaves micro voids which can negatively influence the mechanical
properties of the concrete. The study of air voids created by SAP in concrete is thereby of essence in
advancing the utilisation of HPC and UHPC.
Laustsen et al. [9] and Maire & Withers [10] emphasized the need for proper characterization of air
voids in hardened concrete to include the knowledge of both size distribution and spatial distribution of
the air voids. Characterization of the air voids is noted to adopt linear-traverse method and the
modified point-count method [11, 12]. Both methods adopts 2D observations to describe 3D
structures, hence the limitations of influence of results obtained by sample preparation and hence
inaccuracies in air void volumes determined. The use of X-ray computed tomography (CT-scanning)
being a powerful measuring technique which provides information about the 3D structure of a sample
without any preceding preparation [13] thereby comes in handy for better air void analysis. Information
on the influence of curing age and SAP contents on the air void distribution in concrete and
cementitious materials are also of importance for a proper and appropriate use of SAP as IC agent in
concrete construction.
This paper reports on 3D volume analysis of the air voids in HPC containing SAP as IC-agent using
commercial computer software having little operators influence as recommended by Laustsen et al.
[8] for better output. The concrete samples used for the image analysis were also made to appropriate
sizes to gives a true reflection of the actual pore and void states. It further examines the influence of
hydration period, SAP type, SAP content and binder type on the air void size, sphericity and
distribution.
2
2.1
EXPERIMENTAL INVESTIGATION
Materials
Two sizes of SAP ( 300 m with product label FLOSET CS 27 and 600 m labelled FLOSET CC
27) were used at different SAP content: 0%, 0.2%, 0.3% and 0.4% by weight of binder. The SAP are
thermoset polymers specifically covalently cross-linked polymers of acrylic acid and accrylamide,
neutralised by alkali hydroxide, which according to Schrofl, Mechtcherine, & Gorges [14] have been
proven efficient as internal curing agents in concrete. The absorption capacity of the SAP is shown in
previous work [15] to be 250 g/g in distilled water and 25 g/g (i.e. 2500 %) in cement pore solution
(CPS) for both SAP grain sizes.
A natural sand with minimum particle size of 300 m (i.e. all the particles smaller than 300 m was
removed using the sieving method) having the following physical property: Fineness Modulus (FM =
2.79), coefficient of uniformity (Cu = 2.43), coefficient of gradation (Cc = 1.02) and dust content (0.3%)
of medium sand classification [16] as observed in the preliminary sieve analysis reported in Olawuyi &
Boshoff [17] was used as fine aggregate. 13 mm crushed greywacke stone was used as the coarse
aggregate. OPC CEM I 52.5 N conforming to BS EN 197 [18] was the binder with silica fume, corex
slag and fly ash added as cement extender while Premia 310 (a PCE) supplied by Chryso, was added
as superplasticizer. The composition of the reference HPC mixtures is shown in Table 1.
Table 1: Mix constituents of HPC mixtures
Constituents
M1
Water
125
125
134
155
530
530
540
500
1050
1050
1050
590
1050
590
710
700
Fly Ash
122.5
Corex Slag
122.5
Silica Fume
52.5
52.5
40
40
21
21
16
5.4
0.2
0.2
0.25
0.3
Water/binder ratio
2.2 Methods
Four reference HPC mixtures of different binder combination types (cement, silica fume, fly ash and
corex slag); W/B (M1 & M1D (0.2); M2 (0.25) and M3 (0.3)) and 28-day characteristic strength (fck, cube)
of 70 MPa minimum (i.e. C60/C75 C90/C105 HSC) were made using the method described in Atcin
[19] for HPC with other mixes having varied SAP contents (0.2% ; 0.3% and 0.4%) for the two SAP
sizes (Sp1 and Sp2). Workability and cohesion of the fresh HPC mixtures was determined using the
Slump flow table to ensure consistent workability for all the mixture irrespective of SAP content. The
concrete was cast in 50 mm x 100 mm cylindrical moulds and cured in water at 23 3 oC for
different hydration periods (i.e. 28, 56 and 90 days respectively) in accordance to relevant BS
Standards [2, 20, 21, 22, 23]. The hardened HPC specimens were then placed in the oven at 40 oC
for 30 minutes after removal from curing tank at respective hydration period to make it totally dry
before taken to the CT scanner for analysis. Mix M 1 and M1D are both of the same W/B (0.2); mixture
M1 contains fly ash whereas M1D has corex slag as cement extender. The dry hardened HPC was
subjected to X-ray CT scanning for the determination of the air void distribution. The 3D X-ray images
were then examined and analysed using Avizo Fire, version 8.0 [24] and VG Studio Max 2.2 [25] (both
being commercial computer programmes) to filter and classify the individual voids for determination of
the sizes, distribution and volume analysis of void created by SAP in the HPC with the respective
influence of binder type, water/binder ratio, SAP content and curing age. The CT scanning was also
used to affirm the grain sizes and distribution of the dry SAP particles.
The 3D X-ray images were obtained using a General Electric Phoenix VTomeX L240 X-ray micro
computed tomography scanner (micro-CT). Each concrete specimen was mounted in a less dense
cardboard tube to reduce external influences on the samples during the scan. Reconstruction was
performed with system supplied Datos Reconstruction software and analysis was conducted. The
voxel size was set to 100 m with settings at 170 kV and 150 A for x-ray generation and image
acquisition settings was 500 ms per image. The 3D image of HPC specimen is shown in Figure 1a
while Figure 1b shows the 2D slice image of same.
The VGStudio Max 2.2 analysis require selection of a surface to identify only the voids in the sample
with a defect analysis performed on these voids to determine the size and abundance of the void. The
results from the analysis includes size, abundance, sphericity and volume of the voids
Image analysis using the Avizo Fire 8.0 involved the following steps:
i.
ii.
iii.
iv.
v.
vi.
vii.
viii.
ix.
maintained);
Non-local means filter - to smoothen the data;
interactive thresholding - to colour the pores;
separate objects - to separate touching pores;
label analysis - volume render and data saved and
Sieve analysis.
All the various stages of analysis have minimum human influence except the thresholding aspect.
Details of the method adopted for the 3D volume analysis can be found in recent literatures [10, 26].
The outcome of the analysis was then plotted using histogram chart for the respective HPC mixtures
tested after 28 days of curing and is shown in Figure 6 to 9.
(a)
(b)
Figure 2: 3D Image of separated dry SAP particles with colour indicating sizes classification (a) and
(b) Centrally cropped CT image of dry SAP particles obtained from 3D VGI file
3.1
The SAP particles were observed to be of varied sizes and shapes; they are mostly angular and
irregular in shape and not totally spherical. The grain sizes are noted to be in the range of
0/300 m (Sp1) and 0/500 m (Sp2) when examined under CT scanning (3D) image analysis (Figure
2). These values agree very well with the manufacturers specification of
600 m (Sp2) respectively. Table 2 shows the frequency distribution of the particles (using class
intervals of 25 m) while Figure 3 presents the cumulative volume (%) present for the size classes in
diameter. About 50 % (D50) of the Sp1 particles were lower than 160 m while Sp2 has D50 of 260
m. A close observation of the SAP particles individually (Figure 4) reveals that some particles have
hollow voids within at the dry stage while a sphericity assessment of the particles shows the SAP
particles has average sphericity values of 0.86 (Sp1) and 1.14 (Sp2), hence the larger the SAP size,
the less spherical it becomes.
Sphericity is a measure of the roundness of a shape. A sphere is the most compact solid, so the more
compact an object is, the more closely it resembles a sphere. Sphericity is a ratio and therefore a
dimensionless number. Sphericity s is defined as:
6Vp
DpAp
Sp2
0
22436
133
594
681
449
245
180
113
84
76
56
57
25
26
14
12
8
3
1
0
390
260
110
Figure 3: % cumulative volume present of various particle sizes for Sp 1 and Sp2
Figure 4: CT image of examination of individual SAP particles obtained from a 3D VGI file
3.2
Figure 6 to 9 for the various HPC mixtures after 28 days of hydration reveals that air voids exists in all
the HPC samples irrespective of the SAP content and concrete mixture. The peak of the histogram
were noted to be around the same values (i.e. 225 m 300 m diameter air voids = 0.06 0.141
mm3 pore volume sizes) whereas only a reference mix, M 1D has a peak at 375 m. These can be seen
to refer to air voids created by SAP dry particles of sizes 0 to 100 m; the range within which bulk of
the particle sizes of SAP belong as seen in Table 2. A critical study of histograms further reveals that
the air voids distribution are more and of wider spread in HPC specimen containing SAP. Presence of
micro-air voids in the reference mixes also show that the high concentration of superplasticizer
resulted in air bubbles which could not be totally eliminated by vibration of concrete. SAP addition
however created more air voids in the HPC and these air voids were observed to be well distributed
within the concrete.
M1-28D
M1Sp10.2-28D
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
6000
4000
2000
Frequency
0
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
6000
4000
2000
Frequency
0
Volume (mm3)
(a)
Volume (mm3)
(b)
M1Sp10.3-28D
M1Sp10.4-28D
6000
4000
2000
Frequency
0
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
00
0.
07
58
0.
60
61
2.
04
57
6000
4000
2000
Frequency
0
Volume (mm3)
(c)
Volume (mm3)
(d)
M1Sp20.2-28D
M1Sp20.3-28D
6000
4000
2000
Frequency
0
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
0.
00
00
0.
11
31
0.
90
48
3.
05
36
6000
4000
2000
Frequency
0
Volume (mm3)
(e)
Volume (mm3)
(f)
M1Sp20.4-28D
0.
00
0
0. 0
11
3
0. 1
90
4
3. 8
05
36
6000
4000
2000
Frequency
0
Volume (mm3)
(g)
Figure 5: Histogram Plot of Air Void Distribution of (25 x 25 x 50 mm3) M1 HPC Samples
M1D-28D
M1DSp10.2-28D
3000
2000
1000
0
Frequency
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
0.
00
00
0.
11
31
0.
90
48
3.
05
36
3000
2000
1000
0
Frequency
Volume (mm3)
(a)
Volume (mm3)
(b)
M1DSp10.4-28D
M1DSp10.3-28D
3000
2000
1000
0
Frequency
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
3000
2000
1000
0
Frequency
Volume (mm3)
(c)
Volume (mm3)
(d)
M1Sp20.2-28D
M1DSp20.3-28D
3000
2000
1000
Frequency
0
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
0.
00
00
0.
11
31
0.
90
48
3.
05
36
3000
2000
1000
Frequency
0
Volume (mm3)
(e)
Volume (mm3)
(f)
M1DSp20.4-28D
0.
00
00
0.
11
31
0.
90
48
3.
05
36
3000
2000
1000
0
Frequency
Volume (mm3)
(g)
Figure 6: Histogram Plot of Air Void Distribution of (25 x 25 x 50 mm3) M1D HPC Samples
M2-28D
M2Sp10.2-28D
4000
2000
0
Frequency
(a)
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
0
0. 0
11
3
0. 1
90
4
3. 8
05
36
4000
2000
0
Frequency
Volume (mm3)
Volume (mm3)
(b)
M2Sp10.3-28D
M2Sp10.4-28D
4000
3000
2000
1000
0
Frequency
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
4000
3000
2000
1000
0
Frequency
Volume (mm3)
Volume (mm3)
(c)
(d)
M2Sp20.2-28D
M2Sp20.3-28D
4000
4000
2000
0
Frequency
2000
0
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
0.
00
0
0. 0
11
3
0. 1
90
4
3. 8
05
36
Frequency
Volume (mm3)
(e)
Volume (mm3)
(f)
M2Sp20.4-28D
4000
2000
0
0.
00
0
0. 0
11
3
0. 1
90
4
3. 8
05
36
Frequency
Volume (mm3)
(g)
Figure 7: Histogram Plot of Air Void Distribution of (25 x 25 x 50 mm3) M2 HPC Samples
M3-28D
M3Sp10.2-28D
1500
1000
500
Frequency
0
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
3000
2000
1000
Frequency
0
Volume (mm3)
(a)
Volume (mm3)
(b)
M3Sp10.3-28D
M3Sp10.4-28D
3000
2000
1000
Frequency
0
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
2000
1500
1000
500
Frequency
0
Volume (mm3)
(c)
Volume (mm3)
(d)
M3Sp20.2-28D
M3Sp20.3-28D
3000
2000
1000
0
Frequency
0.
00
00
0.
11
31
0.
90
48
3.
05
36
0.
00
0
0. 0
07
5
0. 8
60
6
2. 1
04
57
2000
1500
1000
500
0
Frequency
Volume (mm3)
(e)
Volume (mm3)
(f)
M3Sp20.4-28D
0.
00
00
0.
11
31
0.
90
48
3.
05
36
2000
1500
1000
500
Frequency
0
Volume (mm3)
(g)
Figure 8: Histogram Plot of Air Void Distribution of (25 x 25 x 50 mm3) M3 HPC Samples
3.3 Influence of SAP contents on Air Void Distribution
The general trend is that SAP void % and total void % (i.e. percentage porosity) increased as the SAP
content increased and also as W/B increased with little variations (Figures 5 to 8). Figure 9 shows that
the SAP void % increased with increase in SAP contents for all HPC mixtures at 28 days irrespective
of the SAP size except for the outliers. The higher the binder (i.e. fines) content the lower the porosity
and hence the better the HPC produced. The reason for the observed variation could be due to the
fact that only single sample of each specimen was used for the CT scanning analysis, further works
using triplicate samples is thereby recommended.
A study of the maximum and the minimum void sizes reveals neither a particular trend nor
consistency. In all the HPC mixtures, the reference mix at 28 days gave maximum void sizes amongst
the largest values (M1 (57.80 mm3); M1D (39.41 mm3); M2 (122.2 mm3) and M3 (50.04 mm3) - Tables 3
to 6). This can possibly explain the variations observed in the percentage porosity as recorded. Some
excess water was trapped within the concrete hence creating large air voids which are not void
created by SAP. These large air voids form part of what was used to calculate total void but were
excluded in the calculation of SAP voids %. The minimum void size in all the concrete samples were
however same value (0.0013 mm3). This is because the CT scanning on the HPC was carried out at
100 m; hence the lowest air voids that can be detected are those above 100 m. The average void
size too did not give a particular trend or consistency. This is because of the presence of some
arbitrary large void sizes which thereby influenced the value of average void size calculated. A study
of the triplicate samples will surely give a better conclusion on the influence of SAP contents and W/B
or mixture type on the air void distribution of HPC.
The optimum SAP content for the HPC mixtures can however be taken as 0.3 (since the outliers as
observed on Figure 9 are mainly noticed at SAP contents higher than 0.3 %). The presence of a high
number of large air voids (1500 mm3) in HPC of higher SAP contents can therefore be responsible
for observed loss in strength and relative low mechanical properties pointed out in previous studies
[27, 28, 29, 15]. HPC made of high W/B definitely has a lesser need for internal curing and hence the
less the demand for SAP as IC-agent. SAP air voids cannot however be said to be detrimental to the
porosity of HPC as SAP voids for all SAP containing HPC mixtures studied lies below 2 - 5% with the
average porosity values all below 3%. This is below the expected SAP voids calculated based on
additional water provided for SAP and also the de-moulded concrete porosity for the HPC mixtures.
The reference mix for the HPC with 0.3 W/B (i.e. M3) gave a total porosity value similar to same
mixtures containing SAP. This can be due to excess air bubbles created by superplasticizer since
concrete at higher W/B has less need for water reducing agents. The mixtures containing Fly Ash and
Corex Slag as cement extenders (M1 and M1D; at W/B of 0.2) however showed a good trend of the
influence of SAP on HPC with the SAP air voids been about 50 % of expected SAP pore content.
The SAP type can be adjudge to influence the air void content in all HPC specimens, as the void
volumes for Sp2 is taken as about double the void volumes in Sp 1. This is because as observed in 3.1
above, Sp2 (0/500 m) is double Sp1 (0/300 m) in size.
3.0
2.5
2.0
Void (%)
1.5
M1Sp1
1.0
M1DSp1
M2Sp1
M3Sp1
0.5
0.0
0
0.1
0.2
0.3
0.4
0.5
5.0
4.5
4.0
3.5
3.0
Void (%)
2.5
M1Sp2
2.0
M1DSp2
M2Sp2
M3Sp2
1.5
1.0
0.5
0.0
0
0.1
0.2
0.3
0.4
0.5
Table 3: Summary of Influence of SAP contents and curing age on void distribution for M 1 HPC
Curing Age Influence
M1-28D Series
SAP pore expected+
De-moulded Porosity++
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
M1-56D Series
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
M1-90D Series
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
Ref
M1
0.00
0.58
35
0.00
1.47
57.8053
0.0013
0.1535
M1
37
0.00
1.68
55.0342
0.0013
0.0287
M1
29
0.00
1.48
60.6563
0.0013
0.0861
M1Sp10.2
3.40
4.39
45
1.25
2.03
23.1448
0.0013
0.0585
M1Sp10.2
37
1.30
2.22
25.5845
0.0013
0.1079
M1Sp10.2
45
1.35
2.21
77.9447
0.0013
0.0794
SAP1
M1Sp10.3
5.01
6.56
48
1.51
2.91
65.5331
0.0013
0.0878
M1Sp10.3
37
1.87
2.68
57.4526
0.0013
0.0656
M1Sp10.3
53
2.21
3.31
55.6584
0.0013
0.0888
M1Sp10.4
6.56
6.66
52
2.77
4.42
49.5119
0.0013
0.0707
M1Sp10.4
64
2.60
4.02
15.7617
0.0013
0.0570
M1Sp10.4
55
2.57
4.40
38.8080
0.0013
0.0878
M1Sp20.2
3.40
2.43
35
2.19
2.53
14.7461
0.0013
0.0554
M1Sp20.2
42
1.68
2.07
46.9377
0.0013
0.0637
M1Sp20.2
39
1.63
2.00
30.2217
0.0013
0.0534
SAP2
M1Sp20.3
5.01
5.67
57
3.05
3.53
11.2816
0.0013
0.1070
M1Sp20.3
67
3.91
4.49
32.8651
0.0013
0.1161
M1Sp20.3
152
3.88
5.31
31.2426
0.0013
0.1664
M1Sp20.4
6.56
6.17
70
4.40
5.06
55.9819
0.0013
0.0556
M1Sp20.4
36
2.23
2.56
121.8050
0.0013
0.0604
M1Sp20.4
51
2.69
3.17
61.0476
0.0013
0.0560
Table 4: Summary of Influence of SAP contents and curing age on void distribution for M 1D HPC
Curing Age Influence
Ref
M1D-28D Series
M1D
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
M1D-90D Series
0.00
0.20
13
0.00
0.82
39.4069
0.0013
0.1085
M1D
25
0.00
1.32
39.5014
0.0013
0.0695
M1D
SAP1
SAP2
M1D Sp10.2
M1D Sp10.3
M1D Sp10.4
M1D Sp20.2
M1D Sp20.3
M1D Sp20.4
3.40
3.99
32
1.60
2.31
41.7455
0.0013
0.0656
5.01
4.47
26
1.92
2.60
17.2391
0.0013
0.0517
6.56
6.38
17
0.73
1.08
26.4097
0.0013
0.0391
3.40
3.52
39
2.71
3.05
22.1718
0.0013
0.0815
5.01
4.96
29
1.70
1.98
23.4150
0.0013
0.1003
6.56
6.39
45
2.65
3.03
14.5798
0.0013
0.0934
M1D Sp10.2
M1D Sp10.3
M1D Sp10.4
M1D Sp20.2
M1D Sp20.3
M1D Sp20.4
21
0.64
1.03
42.2539
0.0013
0.0752
25
1.18
1.62
66.9719
0.0013
0.0716
32
1.89
2.77
31.1374
0.0013
0.0602
21
1.73
1.91
13.1822
0.0013
0.0818
154
3.46
4.92
67.1117
0.0013
0.1977
21
1.47
1.68
31.0256
0.0013
0.0957
M1D Sp10.2
M1D Sp10.3
M1D Sp10.4
M1D Sp20.2
M1D Sp20.3
M1D Sp20.4
No of voids 1500 m
27
29
45
22
47
22
26
SAP Void %
0.00
1.55
1.73
1.86
2.15
2.40
2.45
Total Porosity %
0.86
2.29
2.65
2.63
2.55
2.61
2.69
Max Void Size (mm3)
28.2159
15.2320
35.8571
21.9362
23.8276
17.2884
15.4103
Min. Void Size (mm3)
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
Av. Void Size (mm3)
0.1477
0.0608
0.0817
0.0593
0.0641
0.0784
0.1051
+Expected pore content by volume based on the 25 g/g pore absorption used for provision of additional water
calculated taking the swollen SAP as a spherical substance.
++
Porosity calculated volumetrically using De-moulded density in comparison to designed density.
Table 5: Summary of Influence of SAP contents and curing age on void distribution for M 2 HPC
Curing Age Influence
M2-28D Series
SAP pore expected+
De-moulded Porosity++
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
M2-56D Series
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
M2-90D Series
No of voids 1500 m
SAP Void %
Total Porosity %
Max Void Size (mm3)
Min. Void Size (mm3)
Av. Void Size (mm3)
Ref
M2
0.00
0.17
63
0.00
2.33
122.1950
0.0013
0.1247
M2
49
0.00
2.29
28.6351
0.0013
0.0770
M2
33
0.00
1.78
78.9696
0.0013
0.0913
M2Sp10.2
2.85
2.37
50
2.01
3.05
101.0430
0.0013
0.0640
M2Sp10.2
50
0.93
1.71
93.9300
0.0013
0.0707
M2Sp10.2
47
1.44
2.44
46.8672
0.0013
0.0680
SAP1
M2Sp10.3
4.21
3.98
63
1.91
3.65
52.7768
0.0013
0.1244
M2Sp10.3
70
1.37
3.02
84.8632
0.0013
0.1161
M2Sp10.3
36
1.77
2.60
41.0228
0.0013
0.0648
M2Sp10.4
5.53
5.47
47
1.19
2.22
87.1312
0.0013
0.1199
M2Sp10.4
44
1.14
2.03
34.1548
0.0013
0.0881
M2Sp10.4
67
2.05
3.19
14.3176
0.0013
0.0733
M2Sp20.2
2.85
1.88
98
2.51
3.39
43.9629
0.0013
0.1469
M2Sp20.2
43
1.86
2.23
52.4560
0.0013
0.1293
M2Sp20.2
85
2.19
2.95
24.7034
0.0013
0.2126
SAP2
M2Sp20.3
4.21
4.06
118
3.12
4.19
87.0767
0.0013
0.1907
M2Sp20.3
36
2.00
2.35
49.9551
0.0013
0.0909
M2Sp20.3
40
1.98
2.37
34.7591
0.0013
0.1029
M2Sp20.4
5.53
5.38
157
3.12
4.65
53.5381
0.0013
0.2474
M2Sp20.4
195
2.84
4.72
72.2334
0.0013
0.3734
M2Sp20.4
107
2.89
3.88
28.5593
0.0013
0.1779
Table 6: Summary of Influence of SAP contents and curing age on void distribution for M 3 HPC
Curing Age Influence
Ref
SAP1
SAP2
M3-28D Series
M3
M3Sp10.2
M3Sp10.3
M3Sp10.4
M3Sp20.2
M3Sp20.3
M3Sp20.4
SAP pore expected
0.00
2.64
3.91
5.14
2.64
3.91
5.14
De-moulded Porosity
1.58
3.25
6.00
6.00
3.92
3.56
4.54
No of voids 1500 m
65
50
57
191
171
119
199
SAP Void %
0.00
2.27
2.32
1.94
4.04
4.09
3.33
Total Porosity %
3.54
3.85
4.12
5.73
5.63
5.26
5.23
Max Void Size (mm3)
50.0416
14.2617
20.4162
103.9910
86.8118
53.2107
48.4244
Min. Void Size (mm3)
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
Av. Void Size (mm3)
0.1156
0.0821
0.0930
0.2443
0.1742
0.1576
0.2170
M3-56D Series
M3
M3Sp10.2
M3Sp10.3
M3Sp10.4
M3Sp20.2
M3Sp20.3
M3Sp20.4
No of voids 1500 m
53
43
42
196
84
149
113
SAP Void %
0.00
1.75
1.39
2.23
3.05
3.34
3.75
Total Porosity %
2.10
2.84
2.33
6.05
3.86
4.71
4.83
Max Void Size (mm3)
22.0547
38.5817
46.5664
39.6771
55.8621
60.3435
25.2584
Min. Void Size (mm3)
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
Av. Void Size (mm3)
0.1185
0.0779
0.0915
0.1973
0.1859
0.1790
0.1508
M3-90D Series
M3
M3Sp10.2
M3Sp10.3
M3Sp10.4
M3Sp20.2
M3Sp20.3
M3Sp20.4
No of voids 1500 m
34
35
64
70
51
52
104
SAP Void %
0.00
1.04
1.98
2.06
2.44
2.44
3.19
Total Porosity %
1.98
2.41
3.49
3.85
2.95
2.92
4.15
3
Max Void Size (mm )
31.7151
28.7177
12.1826
71.1845
45.9914
100.9750
26.2220
Min. Void Size (mm3)
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
0.0013
Av. Void Size (mm3)
0.0679
0.1026
0.1134
0.1008
0.1533
0.1634
0.1465
+Expected pore content by volume based on the 25 g/g pore absorption used for provision of additional water
calculated taking the swollen SAP as a spherical substance.
++
Porosity calculated volumetrically using De-moulded density in comparison to designed density.
3.4
Tables 3 to 6 present summary of the result of influence of curing age, SAP type and SAP contents on
the SAP air void distribution of the various HPC specimens. Figures 10 to 13 on the other hand show
the trend of the cumulative small air void volume (i.e. all air voids below 1500 m in size) present in
the various HPC. This was to investigate influence of curing age, SAP type and contents on the
pattern of air void distribution in the respective HPC mixtures. Although a single sample of each
specimen were analysed, a total of 84 HPC specimens were studied using the CT scanner.
The results in Tables 3 and 4 reveal a trend that for M1 and M1D (W/B = 0.2 in reference mix), the total
voids % decreased as the hydration period increased. The SAP voids were also noted to increase as
the SAP size and contents increased at all the respective hydration periods for both HPC mixes. A
closer examination of the number of air voids larger than 1500 m (diameter) as presented in the
tables gives a consistent value range of 30 70 with some few outliers (pink colour highlights in the
tables) while the maximum void sizes was also observed to be of similar value range of 20 70 mm 3
but for two extremes - 11 mm3 and 121 mm3 (blue colour highlights). The pattern of the cumulative
small voids % present in the respective HPC (Figure 9) also gave similar trends with deviation
observed in the specimens marked as outliers (e.g. M1Sp20.3-56D in Figure 10(d); M1DSp10.4-56D and
M1DSp20.4-56D in Figure 11 (c & d)). Effect of large air voids ( 1500 m) was also noted to be glaring
in the total void calculated for these samples. It can thereby be inferred however from this study that
for very low W/B mixes SAP addition made additional internal water available for longer period of
cement hydration leading to possible increase in structure of the cement hydration products and
hence reduction in the voids present.
The HPC with Corex Slag as cement extender (M1D) was however noted to exhibit the lowest number
of large air voids present for all hydration periods. This implies that Corex Slag as a cement extender
enhanced better dispersal of the cement and other fine particles and good utilisation of mixing water
and thereby a possible good early age strength development; a complimentary role to silica fume in
HPC. A study of the particle size distribution, particle structure of the various fine materials and the
general strength development of the HPC mixtures will surely offer good answers to this assertion.
Figures 12 and 13 show similar trends as above in the cumulative small voids present in M 2 and M3
(W/B = 0.25 and 0.3) specimens but with large numbers of void sizes above 1500 m (i.e. large air
voids) and great variation in the value of maximum void size present in these HPC mixtures (pink and
blue colour highlights respectively on the Tables 5 and 6). Void volume values above 70 mm 3 were
noted to be more in these HPC samples with the specimens at 28 Days hydration exhibiting greater
proportion of them while some reference mixes also contain very large air void such as 122 mm 3 in
volume (M2 -28D in Table 5). The numbers of large voids were consistently very high (80 200) in the
M3 mixtures; implying that the additional water provided for the SAP addition got collated to amount to
these large air voids. The SAP voids can however still generally be adjudged to decrease as the
curing age increases despite the higher number of outliers reported for these HPC mixtures. A better
inference on this will emerge if triplicate samples of these specimens are analysed as there are
possibilities that some single specimen examined might be the poor specimen of the particular batch.
The presence of large numbers of air void volumes above 1500 m in these HPC mixtures especially
M3 mixtures even after 90 days of curing (Table 6) is a confirmation that at this W/B ratios addition of
SAP for internal curing purposes might not be required.
The air void content produced by the SAP in all the HPC studied were however noted to be lower than
expected pore content by volume based on the 25 g/g pore absorption used for provision of additional
water (Tables 3 to 6). The result of workability measured using the slump flow table as recorded
revealed that the values did not vary significantly for the various HPC mixtures (i.e. 550 to 600 mm M1 and M1D; 500 to 520 mm - M2; and 450 to 480 mm - M3). The additional water can be taken as
effectively absorbed by SAP in the mixtures; hence the 25 g/g pore absorption is appropriate. It
should be noted that the 25 g/g absorption capacity was arrived at using cement pore solution made
of water and cement (w/c = 5.2) only with no other solid constituents. The aggregates (especially the
coarse aggregates) present in low W/B concrete mixtures can also lead to SAP desorption of part of
the absorbed water in the continuous mixing process of the concrete. This probably contributed to the
large voids presence as observed in the analysis. As discussed in section 3.4 above, the cement
hydration products increasing in size as the curing age increases, also contributes to reduction in the
size of the air voids created by SAP at the fresh state of concrete. Further works on ascertaining the
SAP air void as evaluated using the 3D images at various curing ages using triplicate samples should
offer good explanation to this development.
5.0
5.0
4.0
M1-28D
4.0
M1-28D
3.0
3.0
M1Sp10.2-28D
2.0
Void Content (%)
1.0
M1Sp20.2-28D
2.0
Void Content (%)
1.0
M1Sp10.3-28D
0.0
500 1500
0 1000 2000
M1Sp10.4-28D
Void Diameter (m)
M1Sp20.3-28D
0.0
500 1500
0 1000 2000
M1Sp20.4-28D
Void Diameter (m)
5.0
5.0
4.0
M1-56D
4.0
M1-56D
3.0
3.0
M1Sp10.2-56D
2.0
Void Content (%)
1.0
M1Sp20.2-56D
2.0
Void Content (%)
1.0
M1Sp10.3-56D
0.0
500 1500
0 1000 2000
M1Sp10.4-56D
Void Diameter (m)
M1Sp20.3-56D
0.0
500 1500
0 1000 2000
M1Sp20.4-56D
Void Diameter (m)
5.00
5.00
4.00
M1-90D
4.00
M1-90D
3.00
3.00
M1Sp10.2-90D
2.00
Void Content (%)
M1Sp20.2-90D
2.00
Void Content (%)
M1Sp10.3-90D
0.00
M1Sp20.3-90D
0.00
M1Sp10.4-90D
Void Diameter (m)
0
10
00
20
00
1.00
0
10
00
20
00
1.00
M1Sp20.4-90D
Void Diameter (m)
Figure 10: Influence of Curing Age on Void Content of (25 x 25 x 50 mm3) M1 HPC Samples
4.0
3.5
M1D-28D
3.0
2.5
2.0
Void Content M1DSp10.2-28D
(%) 1.5
1.0
0.5
M1DSp10.3-28D
0.0
500 1500
0 1000 2000
M1DSp10.4-28D
Void Diameter (m)
4.0
3.5
M1D-28D
3.0
2.5
2.0
Void Content M1DSp20.2-28D
(%) 1.5
1.0
0.5
M1DSp20.3-28D
0.0
500 1500
0 1000 2000
M1DSp20.4-28D
Void Diameter (m)
4.0
3.5
M1D-90D
3.0
2.5
2.0
Void Content M1DSp10.2-90D
(%) 1.5
1.0
0.5
M1DSp10.3-90D
0.0
500 1500
0 1000 2000
M1DSp10.4-90D
Void Diameter (m)
4.0
3.5
M1D-90D
3.0
2.5
2.0
Void Content M1DSp20.2-90D
(%) 1.5
1.0
0.5
M1DSp20.3-90D
0.0
500 1500
0 1000 2000
M1DSp20.4-90D
Void Diameter (m)
Figure 11: Influence of Curing Age on Void Content of (25 x 25 x 50 mm 3) M1D HPC Samples
3.5
3.5
3.0
M2-28D
2.5
3.0
M2-28D
2.5
2.0
2.0
1.5
M2Sp10.2-28D
Void Content (%)
1.0
0.5
M2Sp10.3-28D
0.0
500 1500
0 1000 2000
M2Sp10.4-28D
Void Diameter (m)
1.5
M2Sp20.2-28D
Void Content (%)
1.0
0.5
M2Sp20.3-28D
0.0
500 1500
0 1000 2000
M2Sp20.4-28D
Void Diameter (m)
4.0
3.5
M2-90D
3.0
2.5
2.0
M2Sp10.2-90D
Void Content (%)
1.5
1.0
0.5
M2Sp10.3-90D
0.0
500 1500
0 1000 2000
M2Sp10.4-90D
Void Diameter (m)
4.0
3.5
M2-90D
3.0
2.5
2.0
M2Sp20.2-90D
Void Content (%)
1.5
1.0
0.5
M2Sp20.3-90D
0.0
500 1500
0 1000 2000
M2Sp20.4-90D
Void Diameter (m)
Figure 12: Influence of Curing Age on Void Content of (25 x 25 x 50 mm3) M2 HPC Samples
5.00
5.00
4.00
M3-28D
4.00
M3-28D
3.00
3.00
M3Sp10.2-28D
2.00
Void Content (%)
M3Sp20.2-28D
2.00
Void Content (%)
M3Sp10.3-28D
0.00
M3Sp20.3-28D
0.00
0
10
00
20
00
M3Sp10.3-56D
0.00
M3Sp10.4-56D
Void Diameter (m)
M3Sp20.4-28D
Void Diameter (m)
M3Sp10.4-28D
Void Diameter (m)
0
10
00
20
00
1.00
0
10
00
20
00
1.00
M3Sp20.4-56D
Void Diameter (m)
3.50
3.50
3.00
M3-90D
2.50
3.00
M3-90D
2.50
2.00
2.00
1.50
M3Sp20.2-90D
Void Content (%)
1.00
0.50
M3Sp10.3-90D
0.00
0.50
M3Sp20.3-90D
0.00
0
10
00
20
00
0
10
00
20
00
1.50
M3Sp10.2-90D
Void Content (%)
1.00
M3Sp10.4-90D
Void Diameter (m)
M3Sp20.4-90D
Void Diameter (m)
Figure 13: Influence of Curing Age on Void Content of (25 x 25 x 50 mm3) M3 HPC Samples
Influence of SAP addition and curing age on the air voids distribution in HPC have been examined via
a 3D volume analysis using computed tomography (CT) scanner for HPC mixtures of different water/
binder, binder types and SAP types. Also studied with the CT scanner is the dry SAP particles size
distribution, shape and sphericity. The result reveals that
a. CT scanning is a good tool for studying the air voids in concrete, cement pastes and HPC. A
fast approach and representative concrete specimen (50 mm x 100 mm cylinder) enhanced
clear examination of the HPC with little or no modification to the cast specimen.
b. The SAP particles are of varied sizes, mostly angular and irregular in shape and not totally
spherical. The dry SAP particle size distribution analysed using CT scanner (SP 1 - 0/300 m;
c.
SP2 - 0/500 m) agrees with the manufacturers specification (SP 1 300 m; SP2 600 m).
All the HPCs mixtures had micro-air voids present irrespective of SAP contents. SAP created
voids are however more and follows same pattern as the distribution of the dry SAP particles.
d. The HPC mixtures had large volume air voids present possibly being a result of high
concentration of superplasticizer in the HPC. The frequencies of these air voids were high in
HPC of higher water/binders.
e. SAP voids % and total void % in HPC increases as the SAP contents increased, so also as
f.
the W/B increases. These however decreased as the hydration period increased.
SAP addition enhanced a wider distribution of air voids in HPC and does not have detrimental
effect on porosity of concrete for low W/B HPC to limit of 0.3
Further studies on influence of SAP addition on the mechanical properties of very low W/B concrete
(i.e. HPC) containing other cementitious materials and a further CT scanning - 3D analysis of air voids
in similar HPC mixtures using triplicate specimen for an examination of the variability of the results are
thereby recommended.
ACKNOWLEDGEMENTS
We acknowledge the following: Mr. Guillaume Jeanson (Construction Product Manager) SNF Floerger
- ZAC de Milieux, 42163 ANDREZIEUX Cedex FRANCE; Davy Penhard, FEI Visualisation Science
Group; Dr. Anton du Plessis and Stephan le Roux, CT Scanner Unit, Central Analytical Facilities
(CAF), Stellenbosch University, South Africa for the assistance received in materials procurement, use
of facilities, softwares and time input in the analysis.
REFERENCES
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
[10]
[11]
[12]
[13]
[14]
[15]
[16]
[17]
[18]
[19]
[20]
[21]
[22]
[23]
[24]
[25]
[26]
[27]
[28]
[29]
[30]
Cement and Concrete Technology in Africa (ACCTA), Johannesburg, South Africa, 2013. Pp
825-833.
BS EN 197 1 (2000): Cement composition, specifications and conformity criteria for
common cements, BSI, London.
P. C. Atcin: High-performance concrete, Taylor & Francis (1998). .
BS EN 12350 1 (2000): Testing of fresh concrete Sampling, BSI, London.
BS EN 12350 5 (2000): Testing of fresh concrete - Flow Table Test, BSI, London.
BS EN 12390 1 (2000): Testing of hardened concrete - shape, dimension and other
requirement for specimens and mould, BSI, London.
BS EN 1992 1 1 (1992): Eurocode 2 Design of concrete structures General rules and
rules for buildings, BSI, London.
FEI Visualisation Science Group: Avizo Fire (version 8.0) - 3D Analysis software for Scientific
and Industrials Data, (2013) www.vsg3d.com
Volume Graphics: VGStudio Max 2.2- Application software for analysis and visualisation of
industrial computed tomography/ voxel data, (2013) www.volumegraphics.com
A. Du Plessis, B. J. Olawuyi, W. P. Boshoff, S. Le Roux, J. Petren: Simple and fast method for
3D porosity analysis of concrete samples using X-ray computed tomography, (submitted for
publication) (2014).
M. T. Hasholt, M. H. S. Jespersen, O. M. Jensen: Mechanical properties of concrete with SAP part I: Development of compressive strength, in O. M. Jensen, M.T. Hasholt, S. Laustsen (eds.)
Use of Superabsorbent Polymers and Other New Additives in Concrete, PR074, RILEM
Publications, Technical University of Denmark, Lyngby, Denmark, 2010, p. 117--126.
B. Craeye, M. Geirnaert, G. D. Schutter: Super absorbing polymers as an internal curing agent
for mitigation of early-age cracking of high-performance concrete bridge decks, Construction
and Building Materials, 25 (1) (2011) 1-13.
M. T. Hasholt, O. M. Jensen, K. Kolver, S. Zhutovsky; Can superabsorbent polymers mitigate
autogenous shrinkage of internally cured concrete without compromising the strength?,
Construction and Building Materials, 31, (2012) 226-- 230.
B. J. Olawuyi, W. P. Boshoff: 3D void analysis of high performance concrete containing
superabsorbent polymers, submitted for presentation at International Conference on
Application of Superabsorbent Polymers and Admixture in Concrete Construction, Technical
University, Dresden, Germany, September, 2014.