Construction and Building Materials 82 (2015) 192–205

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Construction and Building Materials

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Compressive strength and durability properties of high volume fly ash

(HVFA) concretes containing ultrafine fly ash (UFFA)
Faiz U.A. Shaikh ⇑, Steve W.M. Supit
Department of Civil Engineering, Curtin University, Perth, Australia

h i g h l i g h t s

 The addition of 8 wt.% UFFA improved the compressive strengths of HVFA concretes.
 Durability properties of HVFA concretes are also improved due to addition of 8% UFFA.
 The HVFA concrete containing 8% UFFA exhibited superior durability than ordinary concrete.
 UFFA reduces the porosity of the HVFA matrix and accelerates the pozzolanic activity.
 UFFA produces more C–S–H gel by consuming calcium hydroxide (CH) in HVFA concretes.

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

Article history: This paper presents the effect ultrafine fly ash (UFFA) on compressive strength and durability properties
Received 24 October 2014 of concretes containing high volume class F fly ash as partial replacement of cement. The compressive
Received in revised form 19 February 2015 strengths are measured at 3, 7, 28, 56 and 90 days, whereas the durability properties are measured at
Accepted 24 February 2015
28 and 90 days. Chloride induced corrosion, water sorptivity, volume of permeable voids, chloride ion
Available online 9 March 2015
penetration, chloride diffusivity and porosity of above concretes are measured in durability properties.
Microstructural analysis in terms of thermogravimetric analysis (TGA) is also conducted to identify the
Keywords:
reaction phases of calcium hydroxide in the HVFA matrix containing UFFA. Results show that the addition
Ultrafine fly ash
High volume fly ash
of 8 wt.% UFFA significantly improved the early age as well as later age compressive strengths of ordinary
Compressive strength and HVFA concretes. All above measured durability properties of HVFA concretes are also improved and
Durability in most cases the HVFA concrete containing 32% fly ash and 8% UFFA exhibited superior durability prop-
Corrosion erties than ordinary concrete containing 100% cement. The results also indicate the effectiveness of UFFA
Porosity in producing high packing density and in accelerating the pozzolanic activity to produce more C–S–H gel
Concrete by consuming calcium hydroxide (CH) in HVFA concretes.
Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction which are effective in forming denser matrix leading to higher

For many years, the incorporation of fly ash as partial replace-
ment of cement in concrete is a common practice. The quantity
of fly ash to replace the cement for typical application is limited
to 15–20% by mass of the total cementitious material [1]. As a
by-product of industrial process, the utilization of fly ash has made
some progress in addressing the challenges of sustainable con-
struction. In addition, fly ash has pozzolanic activity which is
attributed to the presence of SiO2 and Al2O3. It reacts with calcium
hydroxide during cement hydration, to form additional Calcium
Silicate Hydrate (CSH) and Calcium Aluminate Hydrate (CAH)
⇑ Corresponding author.
E-mail address: s.ahmed@curtin.edu.au (F.U.A. Shaikh).
strength and better durability [1–3].
The use of high volume fly ash as partial replacement of cement
in concrete has also been studied. The main concern in this regard
is whether or not cement can be replaced by fly ash above the lim-
iting quantity of 15–20% by mass in the concrete. Indeed, the small
percentage is beneficial in optimizing the workability and low cost
but it may not improve the durability to any considerable extent
[4]. On the other hand, due to slow pozzolanic properties of fly
ash particles, low early age strength and durability properties are
observed [5,6]. Moreover, the optimization of high volume fly ash
has raised many arguments and limitations regardless of the fact
that the variation of constituent in fly ash such as alkalis, sulfates,
lime and organics may affect the crystallization and slow down the
pozzolanic reaction [7]. In order to overcome this deficiency, the
incorporation of very small size pozzolanic materials such as silica

http://dx.doi.org/10.1016/j.conbuildmat.2015.02.068
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205 193

fume in concrete containing fly ash has also been studied [8–10]. both early age and long-term strength development, where
Finer and amorphous materials are expected to accelerate the poz- UFFA will compensate the low early strength and class F fly ash
zolanic reaction to improve the early age strength characteristics of will contribute to the long-term strength development due to its
mortars and concretes. slow pozzolanic reaction. However, this hypothesis needs to
Among many micro size pozzolanic materials, ultrafine fly ash be confirmed experimentally before its use in the concrete
(UFFA) is recently developed. UFFA is produced by a proprietary industry.
separation system with a mean particle diameter of 1–5 microns The present paper, therefore, focused on investigating the
and contains 20% more amorphous silica than typical class F fly development of compressive strength from very early age at 3 days
ash [11]. Generally, ultrafine fly ash (UFFA) is produced from pure to later age at 90 days of HVFA concretes containing ultrafine fly
class F fly ash by grinding, and separating the ultrafine particles ash. Various durability properties related to chloride induced cor-
through the air-classification process. The classification system is rosion are also evaluated at 28 and 90 days in above concretes to
performed for the removal of coarse particles by size and weight establish the benefit of using UFFA in HVFA concrete. The
to retain the finer ash fraction. In some cases, this system is benefi- microstructure of paste samples on each mix is also analysed by
cial not only in producing finer materials, but also in reducing the MIP and TGA/DTA results.
carbon content and minimizing the variability of constituents in
typical fly ash [12]. The finer particle size improves the mor-
phology, mineralogy and chemical composition of materials. 2. Experimental details
Moreover, when compared to cement production, the UFFA pro-
2.1. Materials
duction does not require high energy-intensive process thus can
result in a cost saving [13]. The other benefits include reducing The cement used in this study was ASTM type I cement in accordance with the
consumption of natural resources and reducing CO2 emission. On ASTM C150 [19] standard. The commercially available class F fly ash (FA) and ultra-
the other hand, it has been reported that a reduction in the particle fine fly ash (UFFA) were used as partial replacement of cement. The characteristics
of the raw materials based on XRD analysis are shown in Fig. 1. Previous analysis by
size of fly ash increases the amorphous SiO2 content and tends to
the authors also showed that ultrafine fly ash is about 18% more amorphous class F
decrease the amount of SO3 which can prevent the hydration reac- fly ash [20]. The chemical analysis and physical properties of all cementitious mate-
tion of harmful ions in concrete or mortar [14]. rials used in this study are listed on Table 1.
While the UFFA is used to replace cement in concrete, there is
strong indication that an enhancement of strength and higher
long-term durability can also be obtained in HVFA concretes due
to smaller particle size and higher surface area of UFFA.
Therefore, complete hydration reaction can be attained at earlier
ages compared to the ordinary class F fly ash. In addition, the
smaller particles are effective to densify the pores structure and
increase the particle packing to increase the density of concrete
or mortar. However, the UFFA, when present at appreciably high
levels, it tends to increase the water demand as a consequence of
accelerated reaction under fineness and high surface area.
Therefore, typical dosage of UFFA is suggested to be ranged from
8% to 12% of the total binder content [15].
Based on previous experimental research some beneficial
effects have been reported that UFFA was able to enhance the com-
pressive strength when used as partial replacement of cement with
low w/c ratio. Obla et al. [11] reported about 25% and 30% higher
strength at 7 and 28 days, respectively than class F fly ash and ten-
dency to minimize alkali–silica reaction expansion in concrete due Fig. 1. XRD analysis of ordinary Portland cement (PC), class F fly ash (FA) and ultra-
to UFFA addition. Chindaprasirt et al. [16] reported denser matrix, fine fly ash (UFFA) [20].
higher compressive strength and lower total porosity in blended
cement paste containing finer fly ash particles. Hossain et al. [17]
also observed that the replacement of cement with 12% UFFA
Table 1
improved cracking resistance when compared to conventional Chemical composition and physical properties of materials.
Portland cement concrete and silica fume concrete. Subramaniam
et al. [18] observed slight reduction in 1 day compressive strength Chemical analysis Cement (%) Class F Ultrafine
fly ash (%) fly ash (%)
of concrete containing 8% UFFA as partial replacement of cement
with no effect on long-term strength development. They also SiO2 20.2 51.80 73.4
Al2O3 4.9 26.40 17.7
observed higher shrinkage cracking resistance when UFFA contents
Fe2O3 2.8 13.20 4.4
increased from 8% to 12%. Choi et al. [6] also observed that the CaO 63.9 1.61 0.9
compressive strength of concrete increased with increasing fine- MgO 2.0 1.17 0.6
ness of fly ash. The compressive strength was lower than control MnO – 0.10 <0.1
K2O – 0.68 1.03
mixes before 7 days and higher after 14 days. From above investi-
Na2O – 0.31 0.11
gations, it was clear that the improvement of mechanical and dura- P2O5 – 1.39 0.2
bility properties was mainly caused by the fineness of fly ash and TiO2 – 1.44 0.7
became a main factor contributing to the compressive strength. SO3 2.4 0.21 0.2
However, although extensive research has been carried out on Physical properties
ultrafine fly ash blended cement, very few studies evaluated the Particle size 25–40% 6 7 lm 40% of 10 lm Mean size 3.4 lm
effectiveness of ultrafine fly ash in compressive strength develop- Specific gravity 2.7–3.2 2.6 2.0–2.55
Surface area (m2/g) – – 2.51
ment and durability properties of high volume fly ash concrete.
Loss on ignition (%) 2.4 0.5 0.6
The combination of UFFA and class F fly ash is expected to improve
194 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205

2.2. Mixture proportions Q ¼ 900ðI0 þ 2I30 þ 2I60 þ 2I120 þ . . . . . . . . . þ I360 Þ ð1Þ

where, Q = charge passed (coulombs), I0 = current (amperes) immediately after volt-

The experimental program is divided into two parts, the first part investigated
the effects of 8% and 12% (by wt.) replacement of cement by UFFA on the compres-
sive strength of ordinary concrete and HVFA concretes containing 40% and 60% class
F fly ash. The above UFFA contents are selected based on authors’ earlier study
where among various UFFA contents of 5%, 8%, 10%, 12% and 15%, above two select-
ed UFFA contents exhibited the best performance in compressive strength of
cement mortar [20]. Among 8% and 12% UFFA contents, the UFFA content that
exhibited the highest compressive strength in present study is used to evaluate
the corrosion and related durability properties of HVFA concretes containing 40%
and 60% class F fly ash. Detail mixture proportions are described in Table 2.
2.3. Methods
All concretes were mixed in a pan mixer using water to binder ratio of 0.4. The
concrete samples of size 100  200 mm cylinder are cast and demoulded after 24 h.
The concrete specimens were cured in water at room temperature until the testing
days. The mineralogical and microstructural characteristics of the materials were
studied by means of TGA/DTG and MIP.
2.3.1. Compressive strength
The compressive strength of concretes was determined at 3, 7, 28, 56 and
90 days according to ASTM C39 [21] using a loading rate of 0.33 MPa/s. For each
age, three specimens were tested and the mean value of these measurements is
reported.
2.3.2. Water sorptivity
The rate of water absorption (sorptivity) of concrete samples with 50 mm thick
disk was determined at 28 and 90 days according to ASTM C1585 [22]. The principle
of the method is that a specimen has one surface in free contact with water (no
more than 5 mm above the base of the specimen) while the other sides are sealed.
This test determines the rate of absorption of water by hydraulic cement concrete
by measuring the increase in the mass of specimen resulting from absorption of
water as a function of time. The mass of the concrete specimen is regularly mea-
sured to determine the initial absorption from 1 min to the first 6 h. The absorption
(I) is the change in mass divided by the product of the cross-sectional area of the
test specimen and the density of water. The initial rate of water absorption value
(mm/s1/2) is calculated as the slope of the line that is the best fit to I plotted against
the square root of time (s1/2).
2.3.3. Volume of permeable voids (VPV)
This test was conducted to estimate the percentage of voids present in the con-
crete specimens after curing at 28 and 90 days based on ASTM C642 [23] standard.
Volume of permeable voids (VPV) is determined by boiling the 50 mm cut concrete
specimens for at least 5 h in a water tank at 105 °C, weighing the samples in water,
then measuring the percentage of boiled specimen with dried mass and mass in the
water.
age is applied, and It = current (amperes) at t min after voltage is applied.
2.3.5. Mercury intrusion porosimetry (MIP) analysis
This measurement was performed with a PoreMaster series – Quantachrome
instruments, with a pressure ranged between 0.0083 and 207 MPa, and the pore
diameter and intrusion mercury volume were recorded at each pressure point.
The pressures were converted to equivalent pore diameter using the Washburn
equation [25], as expressed in Eq. (2):
2c cos h
d¼ ð2Þ
P
where d is the pore diameter (lm), c is the surface tension (mN/m), h is the contact
angle between mercury and the pore wall (°), and P is the net pressure across the
mercury meniscus at the time of the cumulative intrusion measurement (MPa).
2.3.6. Chloride diffusion
In order to evaluate the chloride content and chloride diffusion coefficient of
various concretes, 100  200 mm cylinder specimens were cast and cured. After
28 days of water curing, two specimens of 50 mm thick were sliced from each cylin-
der and placed in the exposure container containing NaCl solution prepared with a
concentration of 165 ± 1 g NaCl per L of solution. In this study, the specimens were
remained in the NaCl solution for 60 days. Profile grinding was applied to collect
concrete powder samples at depth increments ranging between 1 mm and
16 mm, according to ASTM C1556 standard [26]. Chloride contents of the powder
samples were measured using CL-2000, Chloride Test System, James instruments.
An accurately weighed 3 g sample is dissolved in 20 ml extraction liquid consisting
of a precisely measured concentration of acid. The chloride ions reacted with the
acid of the liquid in an electrochemical reaction. An electrode, with an integral tem-
perature sensor, is inserted into the liquid. The percentage of chlorides is displayed
directly on LCD readout of the apparatus. Chloride diffusion coefficient of each sam-
ple is determined by fitting the data obtained from the chloride profile analysis
according to Fick’s second law of diffusion equation [27].
Fick’s second law of diffusion is a differential equation that describes how the
concentration of a diffusing species varies with time. For one-dimensional diffusion,
the differential equation is as follows:
@cðx; tÞ @ 2 Cðx; tÞ
¼ Da ð3Þ
@t @x2
From a dimensional analysis, it can be shown that the diffusion coefficient, Da,
has unit of length2/time. The chloride penetration distance is measured in mm and
the exposure time is in terms of years.
If it is assumed that there is one-dimension diffusion and that the chloride ion
content at the surface is constant, a solution to Fick’s second law is as follows:
 
x
Cðx; tÞ ¼ C s  ðC s  C i Þ erf pffiffiffiffiffiffiffiffi ð4Þ
2 Da t

where, C(x,t) = the chloride ion concentration at a depth x in mm from the exposed
2.3.4. Rapid chloride permeability test
surface for an elapsed time t in years since the start of chloride exposure, Cs = the
In order to determine the resistance of concrete to the penetration of chloride
chloride concentration at the surface, expressed as percentage (%) of concrete mass,
ion, the rapid chloride permeability test (RCPT) was conducted according to
Ci = the initial (or background) chloride concentration of the concrete, expressed as a
ASTM C1202 [24]. The specimens from each series were tested after 28 and 90 days
% of concrete mass, erf = the error function (a special function related to the integral
curing. After curing, the specimens of 100 mm in diameter and 50 mm in thickness
of a normal probability function), Da = the chloride diffusion coefficient in mm2/year.
which had been conditioned according to the standard were placed in the cells and
subjected to a 60-V potential for 6-h. One of the cells was filled with 0.3 N NaOH
solution while the other filled with 3% NaCl solution. The amount of electrical cur- 2.3.7. Accelerated corrosion test
rent passed through the specimen is measured and the total charge passed (in cou- Accelerated corrosion test was employed to simulate the corrosion of steel rein-
lombs) is used as an indicator of the resistance of the concrete to chloride ion forcement in concrete. The corrosion process was accelerated by impressing an
penetration. The total charge passed through the concrete specimens was calculat- anodic potential between rebar (anode) and steel plate (cathode) to record the var-
ed using the following formula in Eq. (1) [24]: iation of current with time. Concrete specimens of 100  200 mm cylinder were
used after curing in water for 28 days. Deformed steel bars of 16 mm diameter
and 250 mm in length are used and fixed in the center of the specimens after being
cleaned and accurately weighed. The steel bar has an effective cover of 50 mm at
the bottom. The reinforced concrete specimens were immersed in a 3.5% sodium
Table 2 chloride solution in a ‘‘3 days wet’’ and ‘‘4 days dry’’ cyclic regime to accelerate
Mixture proportions of binary and ternary blended concretes. the corrosion. Readings for each type of mixes were taken from two specimens
and recorded every hour using an automatic data taker. The average was calculated
Mix Cement Class F fly Ultrafine Sand Coarse Water
to compute the time of corrosion for the reinforced steel bar.
designation (kg/m3) ash (kg/ fly ash (kg/ (kg/ aggregate (kg/
The schematic of the accelerated corrosion test setup is presented in Fig. 2. The
m3) m3) m3) (kg/m3) m3)
steel bar (anode) of the sample is connected to a 10-V DC power supply. The nega-
PC 400 – – 1100 1184 160 tive terminal of the DC power source is connected to the stainless steel plate (cath-
FA40 240 160 – 1100 1184 160 ode). The impressed current flow is measured regularly and test is stopped when
FA60 160 240 – 1100 1184 160 the initiation of corrosion is detected. A rapid increase in current flow indicates
UFFA8 368 – 32 1100 1184 160 the formation of cracks in concrete samples. In order to measure the weight loss
UFFA12 352 – 48 1100 1184 160 measurement, the corroded steel is retrieved from the broken samples and weight
FA32.UFFA8 240 128 32 1100 1184 160 to be compared with the initial weight after accelerated corrosion test.
FA52.UFFA8 160 208 32 1100 1184 160 After applying the current for a given time, the degree of induced corrosion can
be theoretically calculated according to Faraday’s law as follows:
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205 195

Fig. 2. The accelerated corrosion test set up.

WIapp T
M th ¼ ð5Þ
F
Mth = theoretical mass of rust per unit surface area of the bar (g/cm2), W = equivalent
weight of steel which is taken as the ration of atomic weight of iron to the valency of
iron (27.925 g), Iapp = applied current density (Amp/cm2), T = duration of induced
corrosion (s), F = Faraday’s constant (96,487 Amp-s).
The actual mass of corroded products per unit surface area is measured accord-
ing to Eq. (6) by gravimetric method in accordance with ASTM G1 [28] on rebars
extracted from the concrete by breaking the specimens after the accelerated corro-
sion test

Wi  Wf
M ac ¼ ð6Þ
pDL
where Mac = actual mass of rust per unit surface area of the bar (g/cm2), Wi = initial
weight of the bar before corrosion (g), Wf = weight after corrosion (g) for a given
duration of induced corrosion (T), D = diameter of the rebar (cm), L = length of the
rebar sample (cm).

2.3.8. Differential thermal analysis and thermogravimetric analysis (DTA/TGA)

DTA/TGA analysis measures both heat flow and weight changes in a material as
a function of temperature in a controlled atmosphere. DTA figures the thermal
decompositions of different phases in the paste, while TGA simultaneously mea-
sures the weight loss due to the decomposition of phases. About 50 mg of well-
Fig. 3. Measured slump values of HVFA concretes, concretes containing UFFA and
powdered sample in a 110 lL platinum crucible was heated from ambient to
HVFA concretes containing UFFA.
1000 °C at 20 °C per minute in a nitrogen atmosphere flowing at 100 ml per minute.
Mass and differential temperature data were acquired with respect to furnace
temperature.

compressive strength at all ages compared to that of control con-

3. Results and discussion
3.1. Workability
The effect of ultrafine fly ash on the workability of ordinary con-
crete and concretes containing HVFA is shown in Fig. 3. The work-
ability of concrete is measured in terms of slump value according
to ASTM C1437 [29]. It can be seen in Fig. 3 that the addition of
UFFA decreased the workability and the reduction in slump
increases with increase in UFFA content from 8% to 12% in ordinary
concrete. Similar phenomenon is also observed in HVFA concretes
containing 40% and 60% fly ash. The lower workability of ordinary
concrete and HVFA concretes containing UFFA is due to smaller
particle size and higher surface area of UFFA. Similar behavior is
also observed in the case of HVFA mortar [21].
3.2. Compressive strength
The effect of UFFA on the development of compressive strength
of ordinary concrete and HVFA concretes is shown Fig. 4. It can be
seen that the concretes containing UFFA exhibited higher
crete and concretes containing HVFA. Among different UFFA con-
tents, the highest compressive strength was achieved when
cement was replaced by 8% UFFA. The results show that the
UFFA8 concrete had a compressive strength of 45 MPa, whereas
the compressive strength of control concrete was 29 MPa at
28 days. It was also evident that the UFFA content of 8% significant-
ly improved the early age compressive strength at 3 and 7 days of
ordinary concrete by about 50% and 100%, respectively. The long-
term compressive strength at 90 days of UFFA8 concrete is also
increased by more than 50% compared to control concrete. The rea-
son behind this improvement is due to the small particle and high
amorphous content of UFFA which accelerates the pozzolanic reac-
tion and fills the pores resulting in improved compressive strength.
One of the main purposes of this study was to evaluate the
effectiveness of UFFA on the development of compressive strength
of HVFA concretes both at early age as well as later ages (e.g.
90 days). The effect of ultrafine fly ash on the compressive strength
development of high volume fly ash (HVFA) concretes can also be
seen in Fig. 4. The ultrafine fly ash content of 8% was selected since
it exhibited the highest compressive strength in binary blended
cement concrete. Results show that the addition of 8% UFFA
196 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205
Fig. 4. Compressive strengths of HVFA concretes, concretes containing UFFA and HVFA concretes containing UFFA.
improved the compressive strengths of HVFA concrete containing
40% fly ash at all ages. Similar behavior is also observed in HVFA
concrete containing 60% fly ash, however, the compressive
strength at 28 days and beyond deviated from this trend. The
XRD analysis results, shown in [21], also support this observation
where the drop of calcium hydroxide (CH) peaks at 2theta angels
of 18.04° and 34° can be seen due to addition of 8% UFFA in
HVFA concrete containing 32% fly ash. The change in C–S–H peak
can also be seen in the XRD plot indicating the formation of CSH
due to reaction of UFFA with CH in the pozzolanic reaction. On
the other hand, no significant difference in the CH and CSH peaks
are observed in above concrete at 28 days. The above result is also
consistent with the calculated CH content from the TGA analysis
discussed in following section.
3.3. Water sorptivity
Water sorptivity describes the water ingress into pores of
unsaturated concrete due to capillary suction. It is a function of
porosity including pore volumes and continuity of pores within
the concrete matrix and can be related to permeability. The rate
of absorption (mm) of all type of concrete mixtures at 28 and
90 days are presented in Fig. 5a–d. The best-fit lines in above fig-
ures are based on r2 values of greater than 0.98 for all mixes. It
can be seen that the cumulative volume of water absorbed in the
concrete specimens increased with the square root of time. The
slope of the obtained line defines the sorptivity of different con-
cretes during the initial 6 h of testing. It can be clearly seen that
the rate of water absorption of ordinary concrete is reduced at
28 and 90 days due to addition of 8% UFFA as partial replacement
of cement (see Fig. 5a and c). It is due to fineness, high pozzolanic
activity and the formation of secondary CSH due to reaction of
UFFA particles with CH. According to the summarized sorptivity
values in Fig. 6, the minimum water sorptivity at 28 and 90 days
were 32 and 19 (104 mm/s1/2), respectively for UFFA8 concrete.
The values are about half of the ordinary concrete.
Fig. 5b and d shows that the sorptivity of HVFA concretes is
higher than those containing 8% UFFA with similar w/b ratio
because of high fly ash content. In HVFA concretes containing
UFFA, it can be seen that the FA32UFFA8 concrete exhibits higher
resistance to water absorption by capillary suction than FA40
concrete. Based on the sorptivity values in Fig. 6, the water sorp-
tivity of FA32UFFA8 concrete at 28 and 90 days is about 40% and
60%, respectively lower than that of FA40 concrete. However, the
reduction in sorptivity of this concrete was not as great as of
FA32UFFA8 concrete. In addition, in both HVFA concretes the influ-
ence of UFFA addition on reduction of water absorption due to cap-
illary pores suction after 90 days of water curing was more than
28 days curing, since mature concrete has a more discontinuous
pore system.
The above results show that by combining UFFA in HVFA con-
crete, the capillary absorption of water can be reduced. The reduc-
tion in water sorptivity can be explained as the rapid reaction of
UFFA with CH, thus accelerating the hydration products and
improving the bonding effect between cement paste and aggre-
gate. This process, therefore, improves the density of concrete
due to reduction of pore volume, which is also observed in mercury
intrusion porosity tests discussed in following section.
3.4. Volume of permeable voids (VPV)
Fig. 7 presents the volume of permeable voids of different con-
crete mixes at 28 and 90 days. The VPV is recognized as an impor-
tant property of concrete since it affects the transport mechanism
of aggressive fluids through concrete. As expected, the VPV of
UFFA8 concrete shows a decreasing trend with increase in curing
time. The VPV of UFFA8 concrete at 28 and 90 days is reduced by
nearly between 15% and 20% compared to ordinary concrete. The
effect of UFFA on the VPV of HVFA concretes is also shown in
Fig. 7. It can be seen that the VPV is reduced by about 15–20% in
HVFA concrete containing 40% fly ash and by about 13–14% in
HVFA concrete containing 60% fly ash due to addition of 8% UFFA.
3.5. Rapid chloride permeability
Rapid chloride permeability test (RCPT) was conducted to
investigate the performance of concrete against chloride ingress.
The penetration of chloride ions can reach reinforcing steel bars
and corrode them rapidly. The lower the total charge passed
through the concrete matrix, the higher the resistance to chloride
penetration. ASTM C1202 [24] specifies the rating of chloride per-
meability of concrete based on the charge passed through the
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205 197

Fig. 5. Rate of water absorption of different concretes after 28 days (a and b) and 90 days (c and d) moist curing.

Fig. 6. Effect of UFFA on sorptivity of concrete and HVFA concretes.

specimen during 6 h of testing period. RCPT value of less than 2000 Fig. 8 illustrates the effect of UFFA as a partial cement replace-
coulombs is characterized as low chloride permeability, 2000– ment on the resistance to chloride ion penetration in ordinary con-
4000 coulombs is medium level while higher than 4000 coulombs crete at 28 and 90 days. It can be seen that by combining 8% UFFA
is defined as high chloride permeability [24]. in ordinary concrete a decrease in chloride penetration in terms of
198 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205

Fig. 7. Effect of UFFA on volume of permeable voids of concrete and HVFA concretes.

Fig. 8. Effect of UFFA on volume of chloride ion penetration of concrete and HVFA concretes.

total charged passed from 3443 to 2775 coulombs and from 2916
to 887 coulombs can be achieved at 28 and 90 days, respectively.
At 90 days, the effect of UFFA on chloride ion resistance of concrete
was even more favorable with about 70% reduction in chloride ion
penetration. This clearly indicates that at later ages the chloride
penetration resistance of concrete containing UFFA is significantly
improved. Based on the above classification, the concretes contain-
ing UFFA can be classified as low chloride permeability category
indicating the high corrosion resistance.
In HVFA concretes, the results show that the chloride ion
penetration is increased at both ages compared to ordinary con-
crete. The total charge passed of concrete containing 40% fly ash
(FA40) was 4996 and 3559 coulombs and for concrete containing
60% fly ash (FA60) was 6076 and 4937 coulombs at 28 and 90 days,
respectively (see Fig. 8). In the same figure, the effect of 8% UFFA on
the chloride ion penetration resistance of HVFA concrete is also
shown. The results indicated that when 8% UFFA was added in con-
crete containing 32% fly ash the charge passed decreased sig-
nificantly from 4996 to 2459 coulombs at 28 days, a drop of
about 50% when compared to the reference FA40 concrete without
UFFA. The lower values of charge passed obtained in RCPT test can
be attributed to the change of concrete microstructure and refine-
ment in the pore system due to the use of UFFA in HVFA concretes.
However, based on the coulomb value, the concrete containing 52%
fly ash and 8% UFFA exhibits higher chloride permeability than
FA32UFFA8 concrete indicates connected pore structure. It is also
interesting to see that due to addition of 8% UFFA in HVFA concrete
containing 32% fly ash the chloride ion penetration can be reduced
below the ordinary concrete level at both ages. Furthermore, when
concrete mixes are properly designed in terms of the amount of
UFFA as cement replacement in HVFA concretes, it is possible to
achieve medium chloride ion penetration level as standardized in
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205 199

ASTM C1202 and at later ages this chloride ion resistance is expect-
ed to increase.
3.6. Chloride diffusion
The chloride content profile of different mixes of 28 days cured
concretes subjected to 60 days exposure to NaCl solution is pre-
sented in Fig. 9. The figure shows the measured chloride concentra-
tion at different depths, where the chloride concentration inside
the concrete is measured by percent of binder’s weight. In the chlo-
ride content profile, the rate of chloride diffusion can be deter-
mined from the steepness of the curve. A less steep curve
indicates small difference in chloride concentration between inside
and external surface. On the other hand, the steep curve indicates
slow chloride ion diffusion inside the concrete due to very slow
chloride penetration from the concrete’s surface.
In Fig. 9, it is clearly seen than the steepness of the curves is
high up to about 8 mm from the external surface in both ordinary
concrete and HVFA concretes containing 8% UFFA indicating the
influence of UFFA on the reduction of chloride diffusivity. In order
to quantify the durability performance of the concretes, the surface
chloride concentration (Cs) and the effective diffusion coefficient
(Da) are calculated for each concrete. The procedure used a least-
square best-fit analysis for Crank’s solution to Fick’s law as men-
tioned earlier. The chloride diffusion coefficient of concrete mixes
is presented in Fig. 10. For the ordinary concrete, the calculated
chloride diffusion coefficient is 4.1  1012 m2/s while for concrete
containing 8% UFFA (UFFA8), the diffusion coefficient is 1.28 
1012 m2/s, which is about 70% reduction from the ordinary con-
crete. The chloride diffusion coefficient of HVFA concretes is also
reduced by about 25% to 50% when 8% UFFA is added (see
Fig. 10). It indicates that the UFFA is very effective in reducing
the pore space and its connectivity inside the concrete and there-
fore the chloride diffusion.
3.7. Porosity
Mercury intrusion porosimetry (MIP) analysis is widely used to
evaluate total porosity and size distributions of pores in cement
pastes and concretes. The MIP results of paste samples after
28 days of curing are shown in Fig. 11. It shows the relationship
between the cumulative pore volume and pore diameter in the

Fig. 9. Chloride penetration profile of concrete containing UFFA, HVFA concretes and those containing UFFA at 28 days.

Fig. 10. Effect of UFFA on chloride ion diffusion of concrete and HVFA concretes at 28 days.
200 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205
Fig. 11. Effect of UFFA on porosity of cement paste (a) and HVFA pastes (b) after 28 days of moist curing.
range of 0.01 to 100 lm. Zhang and Islam [30] classified the pores
from 10 to 0.05 lm as large capillary pores, from 0.05 to 0.01 lm
as medium capillary pores and <0.01 lm as gel pores. Gel pores
form as part of CSH and are considered as micro pores. They are
not active in water permeability and do not influence the strength.
However, they influence shrinkage and creep of the concrete. The
capillary pores are partially and completely filled with water and
reduce as hydration continues. Capillary pores affect the strength
and durability of concrete.
Fig. 11a shows the cumulative pore volume of cement paste,
HVFA pastes and pastes containing UFFA cured at 28 days. It can
be clearly seen that the total pore volume particularly capillary
pores of HVFA pastes is higher than pure cement paste and the
pastes containing UFFA. Higher capillary pores of HVFA pastes
can be attributed to the less cement and hence less CSH formed
during hydration reaction and slow pozzolanic reaction of fly ash
in concrete. On the other hand, due to larger surface area and high-
er fineness of UFFA than fly ash, more CSH gel are formed in the
paste containing UFFA, which contributed to the reduction in
capillary pore volume and gel pores (Fig. 11a). It can also be seen
that the addition of UFFA significantly reduced the large capillary
pores of cement paste. The effect of UFFA on porosity of HVFA
pastes is shown in Fig. 12b. It can be seen that by adding 8%
UFFA in paste containing 40% and 60% fly ash the total cumulative
pore volume is reduced by about 36% and 33%, respectively.
Fig. 12a and b show the differential pore size distribution curves
of binary and ternary blended cement pastes obtained by differen-
tiating the cumulative curves in Fig. 11. The region under the curve
represents the concentration of the pores. The value of critical dia-
meter of pore corresponds to the peak point of differential curve.
Fig. 12a shows that the maximum concentration of pores in UFFA
paste is approximately at 0.06 lm and the curve’s peak shifted
towards smaller pore sizes as compared to HVFA pastes and
cement paste. The critical pore diameter of UFFA paste is also con-
centrated between 0.04 and 0.1 lm. The above results also show
that the UFFA paste exhibits not only a lower porosity but also a
finer pore structure than the cement paste. The UFFA paste con-
tains mainly pores with diameter <0.1 lm which restricts the flow
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205
Fig. 12. Effect of UFFA on pore size distribution of cement paste (a) and HVFA pastes (b) after 28 days of moist curing.
of harmful ions into the paste. Since the permeability and penetra-
tion of harmful ions into concrete are affected mainly by the large
and medium capillary pores [30], the incorporation of 8% UFFA is
expected to improve the durability properties of concrete.
In the case of HVFA pastes with 8% UFFA addition, there is a
notable reduction in pore concentration indicating the presence
of UFFA is advantageous for the pores modification. With regard
to FA40 paste sample, the result shows that the cumulative pore
volume is reduced significantly after addition of 8% UFFA.
Fig. 12b shows that the porosity of FA32.UFFA8 is concentrated
around 0.03–0.05 lm which is lower than the concentration of
the pores in FA40 paste. The addition of 8% UFFA shifted the con-
centration of critical pores diameters of HVFA paste containing
32% fly ash from large to medium capillary pores. Similar trend is
also observed in FA52.UFFA8 paste. It is noted that UFFA has a sig-
nificant influence in decreasing the total capillary pores and pore
diameter of HVFA pastes. This suggests that the presence of highly
amorphous UFFA can overcome the negative effect of high volume
fly ash by increasing the reaction degree, filling spaces between
cement and fly ash particles, and increasing the density of
microstructure.
201
3.8. Accelerated corrosion test
Fig. 13 illustrates the corrosion current–time relationship of dif-
ferent types of concretes. The current variation with time was
recorded by using a data taker until the corrosion cracks appear
on the surface of concrete specimens. The figure shows that the
concretes containing UFFA perform better in terms of lower mea-
sured corrosion currents than ordinary concrete. In this study,
the UFFA8 concrete took more than 1000 h to crack. Once the
cracks appeared, oxygen and chloride ions penetrated rapidly
through the specimens and accelerated the corrosion that is evi-
dent in the high currents reading. In HVFA concretes, it can be seen
in Fig. 13b that the time to crack in FA40 and FA60 concretes are
around 350 h, which is much shorter when compared to the crack
initiation time of HVFA concrete containing 32% fly ash and 8%
UFFA (see Fig. 13b). However, the corrosion induced crack
appeared much earlier in HVFA concrete containing 52% fly ash
and 8% UFFA. The longer time of FA32UFFA8 concrete to crack than
FA52UFFA8 concrete is probably due to the higher resistance of the
former concrete to chloride penetration and reduced porosity then
later as discussed in previous sections.
202 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205

Table 3
Corrosion mass-loss measurement of rebar from different types of concretes
containing UFFA.

Mix Initial Final Actual mass Theoretical Percentage of

designation mass mass loss (g/cm2) mass loss (g/ mass loss (%)
(g) (g) cm2)
PC 536 377 2.11 2.80 29.67
UFFA8 532 428 1.37 1.35 19.53
FA40 539 485 0.71 0.84 9.99
FA60 532 467 0.87 0.93 12.31
FA32.UF8 530 492 0.50 0.74 7.16
FA52.UF8 534 469 0.85 0.44 12.09

HVFA concretes. In contrast, the rebars taken from HVFA concretes

containing UFFA are almost free from corrosion as indicated by a
reduction in the weight loss of rebar.
The cumulative theoretical mass loss and the actual mass loss of
rebar of each sample are also tabulated in Table 3. The mass loss
measurement is known as the most reliable method to investigate
the degree of corrosion. Based on the results obtained, the mass
loss of rebar in ordinary concrete was higher than that of UFFA8
concrete. It is also shown that the ordinary concrete lost an esti-
mated 29.67% of its steel reinforcement while the UFFA concrete
lost about 19.53%. The better corrosion resistance of HVFA concrete
specimens containing 8% UFFA is also confirmed from the actual
mass loss where the FA32.UFF8 and FA52.UFFA8 concretes reached
about 7.16% and 12.09% steel loss (approx. 13% and 9% lower than
FA40 and FA60 concretes, respectively). It indicates that the pres-
ence of UFFA reduced the corrosion of rebar in HVFA concretes.

3.9. Differential thermal analysis (DTA) and thermogravimetric

Fig. 13. Effect of UFFA on chloride induced corrosion of concrete (a) and HVFA
concretes (b).
Fig. 14 shows the actual corrosion of steel in HVFA concretes
and those containing 8% UFFA after the accelerated corrosion test.
Significant corrosion can be seen on the surface of the rebars in
analysis (TGA)
The results of DTA/TGA analysis of HVFA cement paste contain-
ing 40% fly ash and that containing 8% UFFA after 3 and 28 days of
curing are shown in Fig. 15. From DTA analysis, the V-shape of the
DTA curve refers to rapid loss of weight followed by rapid gain in
weight under endothermic process. Endothermic process is a pro-
cess or reaction in which the system absorbs energy from the

Fig. 14. Corrosion status of HVFA concrete containing 40% and 60% fly ash and that containing UFFA (areas with significant corrosion are shown in circles).
 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205
Fig. 15. TGA/DTG values of concrete containing UFFA and HVFA concretes containing UFFA measured at (a) 3 days and (b) at 28 days.
surroundings in the form of heat [31]. Several peaks can be detect-
ed in the DTA curves. The peak between 105 and 420 °C represents
the mass loss of combined water due to dehydration of calcium
silicate hydrate, aluminate hydrate and ferroaluminate hydrate,
between 420 and 540 °C corresponds to the dehydration of calcium
hydroxide [32].
In Fig. 15, the DTA curves showed two major endothermic peaks
at 103 °C and 462 °C, corresponding to the dehydration of calcium
silicate hydrate (CSH)/ettringite (AFt) and calcium hydroxide (CH),
respectively. In addition, the AFt/CSH phases can also be identified
by observing the decomposition of hydration products within the
temperature range of about 62–157 °C. In Fig. 15a, when
FA32UFFA8 paste is compared with FA40 paste, it can be seen less
weight loss of CH in FA32UFFA8 paste compared to FA40 paste at
470 °C indicating the CH consumption turns into CSH. However,
since the weight loss from unbound water is lost between
50–200 °C overlapped with the weight loss from CSH gel thus it
is impossible to accurately determine the amount of CSH formed
between them. The TGA curves also show similar pattern to
explain that UFFA participates in the hydration process of the
203
system. TGA is defined as the technique whereby the mass of a
substance in a heated environment is recorded at a controlled rate
as a function of time or temperature [33]. In this study, TGA curves
indicate the changes in mass of pastes due to heating from room
temperature to about 1000 °C. This analysis allows the estimation
of CH from the weight losses in paste samples. Based on the figures,
the weight loss due to the dehydroxylation of CH can be observed
at temperature range between 400 and 500 °C. The calcium
hydroxide (CH) content thus can be calculated according to
Taylor’s formula as follows [34]:
MWCH
CH ð%Þ ¼ WLCH ð%Þ  ð7Þ
MWH2 O
where, WLCH is the weight loss during the dehydration of CH as per-
centage of the ignited weight (%), MWCH is the molecular weight of
CH, MWHO is the molecular weight of H2O.
From Fig. 16, the calculated CH content of HVFA paste contain-
ing 8% UFFA is approximately 7.52% and 6.62% at 3 and 28 days,
respectively which is much lower than the CH content of FA40
paste. It also can be seen that the amount of CH decreased in
204 F.U.A. Shaikh, S.W.M. Supit / Construction and Building Materials 82 (2015) 192–205
Fig. 16. Calculated calcium hydroxide (CH) contents of HVFA concrete and that
containing UFFA at 3 and 28 days.
HVFA pastes due to the addition of UFFA. This could be due to the
reactivity of UFFA in HVFA paste and the consumption of CH by the
pozzolanic reaction.
4. Conclusions
The following conclusion can be drawn from the obtained
experimental results:
1. The concrete containing 8 wt.% UFFA yielded the highest
compressive strength at all ages. The early age compressive
strength of HVFA concretes is also improved due to addition
of 8% UFFA. Most significant improvement of about 200% is
observed in HVFA concrete containing 52% fly ash and 8%
UFFA at 3 days.
2. The addition of 8% UFFA, also improved the long term
(90 days) compressive strength of ordinary concrete by
about 55% and that of HVFA concrete containing 32% fly
ash by only about 10%.
3. Water sorptivity of ordinary concrete containing 8% UFFA
was about 50% and 45% lower at 28 and 90 days, respectively
than the ordinary concrete. The use of 8% UFFA in HVFA con-
crete reduced the sorptivity of 28 and 90 days cured HVFA
concrete by about 35% and 50%, respectively. This is an indi-
cation that the 8% UFFA addition in HVFA system forms a fin-
er pore structure than HVFA paste alone.
4. The volume of permeable voids of concrete containing 8%
UFFA is decreased by 15–20% compared to Portland cement
concrete. On the other hand, the addition of 8% UFFA in
HVFA concrete containing 32% fly ash reduced the VPV by
about 15–23% compared to the FA40 concrete.
5. It was also found that the replacement of 8% Portland
cement with UFFA decreased the chloride ion permeability
of Portland cement concrete by approximately 18% and
65% at 28 and 90 days, respectively. Additionally, the bene-
fits of adding 8% UFFA were also observed in HVFA concretes,
where about 49–68% and 8–34% reductions in chloride ion
penetration of HVFA concretes containing 40% and 60% fly
ash, respectively.
6. The chloride diffusion coefficient of cement concrete is also
reduced by about 69% due to addition of 8% UFFA. The chlo-
ride diffusion coefficient of the high volume fly ash concretes
containing 8% UFFA were about 50% and 25% lower than
FA40 and FA60 concretes, respectively.
7. The mercury intrusion porosimetry (MIP) analysis results
showed that the addition of 8 wt.% UFFA in ordinary con-
crete and HVFA concretes decreased the total capillary
porosities and shifted the pore distribution towards smaller
pore sizes.
8. The concrete containing UFFA also exhibited better corro-
sion resistance in terms of smaller measured corrosion cur-
rents with respect to time when compared to cement
concrete. The UFFA8 concrete took more than 1000 h for
the corrosion cracks to appear. Similar results are also
observed in the case of concrete containing 32% fly ash and
8% UFFA.
9. The mass loss of rebar due to corrosion in cement concrete is
about 29.67% while in UFFA8 concrete loss is about 19.53%.
The addition of 8% UFFA also showed better corrosion resis-
tance in terms of about 29% and 8% reduction in mass loss in
HVFA concretes containing 40% and 60%, respectively.
10. From the microstructure and phase identification point of
view, the MIP and DTA/TGA analysis confirms that the incor-
poration of 8% UFFA reduced the CH content and decreases
the total capillary porosities and pores diameter which can
prevent the harmful chloride ions transport leading to corro-
sion of rebar and deterioration to the ordinary and HVFA
concretes.
Acknowledgement
Authors acknowledge fly ash Australia for donating class F fly
ash and ultrafine fly ash used in this study.
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