International Journal of Advanced Research in Engineering and Technology (IJARET)

Volume 12, Issue 2, February 2021, pp. 106-118 Article ID: IJARET_12_02_010
Available online at http://www.iaeme.com/IJARET/issues.asp?JType=IJARET&VType=12&IType=2
ISSN Print: 0976-6480 and ISSN Online: 0976-6499
DOI: 10.34218/IJARET.12.2.2020.010

© IAEME Publication Scopus Indexed

ACID AND SULPHATE RESISTANCE OF NANO

SILICA RUBBERIZED ENGINEERED
CEMENTITIOUS COMPOSITE
Inthiran Mahendran
Department of Civil and Environmental Engineering
Universiti Teknologi PETRONAS
Bandar Seri Iskandar, Perak, Malaysia

Bashar S. Mohammed
Department of Civil and Environmental Engineering
Universiti Teknologi PETRONAS
Bandar Seri Iskandar, Perak, Malaysia

Sani Haruna
Department of Civil and Environmental Engineering
Universiti Teknologi PETRONAS
Bandar Seri Iskandar, Perak, Malaysia
Civil Engineering Department
Faculty of Engineering
Bayero University, Kano, Nigeria

M. M. A Wahab
Department of Civil and Environmental Engineering
Universiti Teknologi PETRONAS
Bandar Seri Iskandar, Perak, Malaysia

ABSTRACT
The main objective of this study is to determine the acid and sulphate resistance of
Engineered Cementitious Composite (ECC) incorporating crumb rubber and nano
silica. Response Surface Methodology (RSM) is utilized to obtain 13 mix design with
the percentage of crumb rubber ranging from 0% to 6.035%. The percentage of nano
silica in the mixture are ranging from 0% to 4.83%. PVA fibers are kept at a constant
percentage of 2% to avoid balling effect. Four laboratory tests were used for this
investigation, which are compressive strength, acid resistance sulphate resistance, and
efflorescence. The samples were evaluated for residual compressive strength. The
Response Surface Methodology (RSM) technique was employed to establish predictive
responsive models and multi-objectives. The optimization results of the prediction

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 Acid and Sulphate Resistance of Nano Silica Rubberized Engineered Cementitious Composite

model were used to achieve the optimal solution variables. Nano silica has the ability
and properties to overcome the limitation of crumb rubber incorporated ECC with the
optimum dosage. Furthermore, rubberized ECC with nano silica has better chemical
attack resistance (acid attack, sulfate attack and efflorescence) in comparison with
normal concrete.
Key words: Acid resistance, Cementitious composite, Crumb rubber, Nano silica,
sulphate resistance.
Cite this Article: Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and
M. M. A Wahab, Acid and Sulphate Resistance of Nano Silica Rubberized Engineered
Cementitious Composite, International Journal of Advanced Research in Engineering
and Technology (IJARET), 12(2), 2021, pp. 106-118.
http://www.iaeme.com/IJARET/issues.asp?JType=IJARET&VType=12&IType=2

1. INTRODUCTION
Engineered cementitious composite (ECC), is a class of ultra-ductile composite that is used as
a construction material [1]. Categorized as a High-Performance Fiber Reinforced Concrete
(HPFRC), ECC is much more durable than other concretes. Often used in structures that are
subject to cyclic or repetitive loading, ECC is a highly durable material. ECC prevails as a
worthy material to be used in various climates regardless of weather or temperature and in
various alkalinities. ECC is rapidly burgeoning as a standout material in the construction of
high rise buildings and pavements as a result of its remarkable ductility and durability [2, 3].
The behavior of ECC materials under aggressive environment is a significant part of this study.
Aggressive conditions can cause surface deterioration and degradation in concrete and ECC.
Degradation in mechanical properties of concrete such as, strength and Young's modulus. The
other type of damage is the spalling impact, which results from the interior pliable pressure
initiated by the vapor weight. Spalling can be dangerous or be a slow decrease of the concrete
segment. Due to the explosion during fire accidents, the public inside and nearby the structure
are at a higher risk of serious injuries or even death. Therefore, crumb rubber is introduced to
be incorporated with ECC to reduce the effect of spalling and explosion [4]. This is primarily
because the rubber leaves room for water vapour to escape after melting at 170 ° C and tends
to release the pore water pressure and therefore reduce the damage to the hardened concrete.
Crumb rubber (CR) are from waste tires are utilized in concrete to produce rubbercrete for the
construction industry.
Tiny rubber particles ranging in size from 0.075 mm to 4.75 mm are regarded as fine crumb
rubber aggregates. CR represents a part of the aggregate in the concrete mix in the concrete
mix, [5]. Crumb rubber is non-biodegradable products of recycling scrap tires. A shredder or a
cracker mill will be used for a 75 µm to 4.75 mm reduction with the steel, fibers dust and any
contaminants removed, leaving only the rubber particles[6]. Moreover, CR has lower specific
gravity, bulk density, strength, and stiffness compared to fine aggregates [7]. Crumb rubber
could repel water and trap air, which contributes to a decrease in the strength of the rubberized
concrete. Crumb rubber is known to have hydrophobic properties which leads to water particles
to repel and air to consequently be trapped on the surface [8, 9]. If the rubber content increases,
the air content in the rubberized concrete increases. [10]. This leads to the mechanical strength
of the rubbercrete to decrease as the CR content increases [11]. The trapped air on the surface
of the CR raises the thickness of the interfacial transition zone ( ITZ) and causes poor interaction
with the hardened substrate. [12]. Rubbercrete has its drawbacks in terms of strength and
cement matrix bonding. This is where the nano silica plays an important role to increase the
rubbercrete compressive strength and feasibility in the construction industry. Research have
shown that the strength of concrete can be increased with the addition of nano silica. Many

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 Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and M. M. A Wahab

factors contribute to the durability of concrete and chemical attack has a significant impact on
the durability factor. The penetration of different chemical into concrete member may lead to
failure such as strength-loss, cracking, and corrosion of the cement paste of concrete [9, 13].
Nano silica has the ability to fill in the voids between rubber particles and cement aggregates
in the concrete, thus increasing the rigidity [14]. Nano silica (NS) propelled by nanotechnology
can top off the nano-measure porosity of the ITZ. NS helps reinforcing the bond and robustness
of the ITZ between concrete framework and totals, in this way altogether improving the strength
[15]. Moreover, the incorporation of NS in rubberized concrete blends will upgrade the
microstructure by refining the pore framework and densifying the ITZ between the aggregate
and the paste [11, 16, 17].
In terms of durability, several vital factors must be taken into consideration such as its
resistance to chemical attack, water permeability and porosity. The deterioration of concrete
members exposed to hostile sulphuric acid environments is a critical issue of resilience that
influences the efficiency of the life cycle of critical civil infrastructure for acid attack. Acids
found in ground water or wastewater in the atmosphere could decrease strength and corrode
concrete [18]. In addition, concrete buildings in commercial areas are vulnerable to corrosion
owing to acid rain, a major component of which is sulphuric acid. For sulphate attack, the
gypsum present in the concrete it reacts with mono sulfates to produce ettringite. Ettringite
formation is the cause of most of the expansion and disruption of concrete structures involved
in the sulphate attack. This can extensive cracking, expansion and reduction of cement matrix
bond [19]. Efflorescence occurs on the surface of porous building materials as a predominantly
white and thin, foggy salt deposit. Efflorescence is caused when soluble salts and other water
dispersible materials come to the surface of concrete and mortars. The basic role of water is
clear as it is required for disintegration of parts of the blooming salt, just as for their passage
between block, concrete and mortar joint, and, at long last, to the workmanship surface [20].
Response surface methodology (RSM) was employed in this study to study the behaviour
of ECC under aggressive medium. Using careful design of experiments, the main purpose is to
optimize a response (output variable) which is influenced by various independent variables
(input variables). RSM was used in many past researches and studies because of its efficiency
and advantages [16, 17, 21, 22]. Response surface methodology and multi-target enhancement
were successfully utilized to improve the mechanical strength, and deformation properties of
the newly developed nano silica-modified [11, 23]. Acid attack, sulphate attack and
efflorescence are the types of chemical attacks focused in this study.

2. MATERIALS & TEST METHODS

2.1 Materials
In this experiment, ECC with a typically common mix design is used except with the addition
of polyvinyl alcohol as well as crumb rubber. The ECC mix used in this study consists of fine
aggregates (4.75mm / passing No. 4 sieve), Portland Cement, Fly Ash, Water, Superplasticizer,
Poly-vinyl Alcohol fibres (Constant 2%), Crumb rubber (0% - 6.035%) and Nano Silica (0% -
4.83). Fine aggregates generally consist of natural sand or crushed stone with most particles
passing through a 3/8-inch sieve during sieve analysis. Water is one of the main components in
concrete. The water/ cement ratio affects many aspects of the concrete such as strength,
durability and ductility. Superplasticizers are admixtures included for reduction of water to
cement ratio or to lower the settling rate of the concrete. This will maintain the workability
properties of the mix. It can also improve the workability of the cement mix. PVA fiber is used
as reinforcing materials for cementitious composites such as ECC.

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 Acid and Sulphate Resistance of Nano Silica Rubberized Engineered Cementitious Composite

2.2 Testing Procedures

Four laboratory tests were used for this project which are compressive strength in accordance
with (BS 1881: Part 116:1983), Durability test resistance against Acid Attack (ASTM C642),
concrete deformations exposed to Sulfate Solution (ASTM C1012) and Efflorescence (ASTM
C67). For each mix, 9 cubes with dimension of 50mm x 50mm x 50mm will be prepare for
compressive strength test. The cube will be undergoing compressive strength test after being
immersed in curing tank for 3 days, 7 days and 28 days. After removing from the curing tank,
the surface of the concrete need to be wiped and weight it before placed on the testing machine.
ECC cube sizes of 100 mm x 100 mm x 100 mm were prepared for an acid resistance
evaluation. The specimens were cast and cured in moulds for 24 hours and were then removed
from the moulds and held for seven days in a vessel. After seven days, all specimens were kept
in the air for a steady weight of 2 days. The specimens are then weighed and drenched for four
weeks in a 5% sulphuric corrosive (H2SO4) solution. The acidic media pH estimate was at 1.2.
The pH value was periodically tested and held at 1.2. The samples are removed and washed in
running water, kept in the atmosphere for two days for steady weight after 30 days of immersion
in the corrosive arrangement, and the weight loss rate was calculated.
For Sulfate attack test, the specimens were restored in lime water alongside solid shape tests
after demolding. Introductory length readings of the specimens were taken utilizing a standard
comparator before submerging them in 5% sodium sulfate solution to assessing the sulfate
obstruction of the examples in each kind of arrangement as shown in Figure 1. The length
estimations were taken at standard interims of time until 30 days (∼ 1 month) and the extensions
were determined to utilize the equation indicated in the test technique.

Figure 1 Sulphate attack test

For efflorescence test, the samples were partly submerged in distilled water to a depth of
about 25.4 mm for 7 days in the drying room. The specimens were spaced by at least 2 in. (50.8
mm), prior to testing the specimens were dried in an oven for 24 hours. Visual observation was
carried out on all the samples, and comparison was made from each pair of samples. All four
faces of each samples were observed from 3 m under an illumination of not less than 538.2 l
m/m2 by an observer with normal vision. The specimens are then be examined for efflorescence.
It is to be reported as “Nil”, “Slight”, “Moderate”, “Heavy”, or “Serious”.

2.3 Mix Design

In this investigation, the role of RSM is essential as it is used to produce the design mixtures.
Table 1. Shows the ECC mixtures with variable percentages of CR and NS. The substitutions
of the components were made by volume. As seen in the mix design table above, the crumb
rubber percentage ranges from 0 to 6.035 % while nano silica percentage ranges from 0 to
4.83%. It is observed that runs 8 to 10 has similar crumb rubber and nano silica percentage.

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 Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and M. M. A Wahab

This is because the crumb rubber of 2.5 % and the nano silica percentage of 2 % are the most
significant during RSM optimization, so replication is important for data and results reliability.

Table 1. Mix design from RSM

Crumb rubber in % (partial Nano-silica in % (added in
Run replacement with sand by terms of cement)
volume)
1 0 4
2 0 0
3 2.5 2
4 6.035 2
5 2.5 2
6 5 4
7 2.5 4.83
8 2.5 2
9 2.5 2
10 2.5 2
11 0 2
12 2.5 0
13 5 0

3. RESULTS AND DISCUSSION

3.1 Compressive Strength
The compressive strength development of the nano silica modified ECC is shown in Figure 2.
As shown in Figure 2, the mix with the highest compressive strength, which is mix 7, has the
highest percentage of NS and low percentage of CR. The mix with the lowest compressive
strength, which is mix 13, has high percentage of CR and low percentage of NS. This is because
crumb rubber has the tendency to repel water and entrap air leads reduction in strength of the
concrete [8]. This can increase the ITZ thickness cause poor bonding between concrete
particles. On the other hand, nano silica is introduced to overcome the limitations of crumb
rubber incorporated ECC. Nano silica inspired from nano technology can fill up the nano-size
porosity of the ITZ. Nano silica assists in strengthening the bond and compactness of the ITZ
between cement matrix and aggregates, thus significantly improving the strength [15].

Figure 2. Compressive Strength development of nano silica modified ECC

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 Acid and Sulphate Resistance of Nano Silica Rubberized Engineered Cementitious Composite

3.2 Acid Resistance

The acid resistance test for all the 13 mixtures was shown in Figure 3. Mix 13 has the highest
weight loss after 28 days while mix 7 has the lowest weight loss. This is because mix 7 has high
percentage of nano silica and low percentage for crumb rubber which makes the concrete high
strength and compact with less voids between cement matrixes. However, mix 13 has high
percentage of CR and low percentage of nano silica which leads to reduction in strength of the
ECC and high porosity due to the presence of voids in the ECC. Concrete is exposed to acid
attack because of the alkaline elements of the concrete. The reaction between acid and the
calcium compounds in the concrete will form soluble calcium. Furthermore, these salts cause
loss of weight and cohesion of the cement paste when leached. A visual inspection of concrete
that experience acid attack proves the corrosion of the cement paste because of the surface
dissolution of cement paste exposing aggregates. Figure 3b shows the weight loss of ECC from
mix 6 after been exposed to 5% sulfuric acid for 28 days.

a b

Figure 3. (a) Average Weight Loss of ECC (b) Surface deterioration

3.3. Sulphate Resistance Test

As shown in Figure 4, the lowest expansion after 28 days of sulfate attack was obtained by M3
mixture compared to other mixes while mix 4 has the highest expansion after 28 days. This is
because mix 3 has high percentage of nano silica and low percentage for crumb rubber which
makes the concrete high strength and compact with less voids between cement matrix. This
makes it difficult for the gypsum present in the concrete to react with mono sulphates to form
ettringite. Ettringite arrangement is viewed as the reason for most of the extension and
disturbance of solid structures associated with the sulfate attack [24-26]. Thus, leads to further
cracking, expansion and reduction of cement matrix bond. However, mix 11 has high
percentage of crumb rubber with low percentage of nano silica which causes the concrete to
have more voids and high porosity. This enables the ettringite to form with ease. Moreover,
rubberized ECC with nano silica has better sulphate attack resistance compared to conventional
concrete as the highest expansion is only 0.066%. For conventional concrete, immersion in 5%
of sodium sulfate result in about 0.8% expansion in volume of the conventional concrete
samples [19, 27]. Therefore, rubberized ECC with nano silica has better sulphate attack
resistance.

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 Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and M. M. A Wahab

Figure 4 Expansion due to sulfate attack after 28 days.

3.4. Efflorescence Test

Efflorescence occurs when salts are dissolved in moisture inside the concrete. Water acts as a
carrying agent of the salt to the surface of the wall. When water evaporates it leaves the salt as
a small crystals deposit. Efflorescence has minimal impact or effect to the concrete in terms of
compressive strength [28]. Efflorescence are usually caused by mix proportion, insufficient
curing, poor compaction of the concrete and atmospheric conditions that cause a rapid drying
out of the concrete. However, fly ash in the mix reduces the effect efflorescence [28]. As shown
in the Table 2, the majority of mixtures have light efflorescence. Similarly, heavy salt deposit
was noticed for M1 and M6 mixtures which is associated to the atmospheric conditions.

Table 2. Efflorescence test results

Mixtures Degree of salt deposit
M1 Heavy
M2 Light
M3 Moderate
M4 Moderate
M5 Light
M6 Heavy
M7 Light
M8 Moderate
M9 Light
M10 Light
M11 Moderate
M12 Light
M13 Moderate

3.5. Analysis of Variance

Response surface methodology (RSM) is a compilation of analytical model-building
mathematical and statistical techniques. The primary objective is to optimize a response (output
variable) that is affected by different independent variables by careful design of experiments
[29, 30]. The Anova analysis showed a dependable assertion in the prediction of the
compressive strength, acid attack and sulfate attack. For every model, the predicted R2 is in

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 Acid and Sulphate Resistance of Nano Silica Rubberized Engineered Cementitious Composite

sound concurrence with the adjusted R2 on the grounds that the contrast between them was kept
up at beneath 0.2. Besides, the satisfactory exactness of the flag to-commotion proportions was
well over 4 with affirmation that the models can be employed to explore inside the client
characterized configuration space in the RSM. The Anova for all the responses (compressive
strength, acid attack and sulfate attack) considering a significant level of 5% (p < 0.05) are
displayed in Table 3.
The equation in terms of actual factors is determined and can be used to make predictions
about the response for a given levels of each factor. The equation as far as genuine variables
can be utilized to make expectations about the reaction for given dimensions of each factor.
Here, the levels ought to be indicated in the first units for each factor. These equations ought
not be utilized to decide the overall effect of each factor since the coefficients are scaled to suit
the units of each factor and the catch is not at the focal point of the plan space. The 2-
dimensional contour plot is used to show the interaction between the independent variables and
their effect on the response variables [31]. As shown in Figure 5a, the contour plot of a
compressive strength model is represented by an elliptical shape which indicate good
interaction between the crumb rubber and nano silica, the interaction in Figure 5c is slightly
lower than that of Figure 5a, while the interaction is perfectly excellent for Figure 5e which
represent the expansion model. Similarly, 3-D graph shown in Figure 5(b, d, f) indicates the
synergistic effect between crumb rubber and nano silica for all the responses.

Table 3. Anova analysis

Responses Factors S. S M.S F-Value P-Value Comments
Compressive strength (MPa) Model 156.95 31.39 15.40 0.0012 significant
A-Crumb
25.06 25.06 12.30 0.0099
rubber
B-Nano silica 92.5 92.50 45.39 0.0003
AB 4.95 4.95 2.43 0.1631
A2 14.74 14.74 7.23 0.0311
B2 1.35 1.35 0.6616 0.4428
Residual 14.27 2.04
Lack of fit 10.74 3.58 4.07 0.1044 insignificant
Weight loss (%) Model 264.81 52.96 37.33 <0.0001 significant
A-Crumb
10.93 10.93 7.70 0.0275
rubber
B-Nano silica 193.94 193.94 136.68 <0.0001
AB 3.69 3.69 2.60 0.1510
A2 4.14 4.14 2.92 0.1312
B2 11.66 11.66 8.22 0.0241
Residual 9.93 1.42
Lack of fit 8.07 2.69 5.76 0.0620 insignificant
Sulfate attack: average
Model 0.0050 0.0010 33.18 < 0.0001 significant
expansion (%)
A-Crumb
0.0011 0.0011 37.41 0.0005
rubber
B-Nano silica 0.0013 0.0013 44.09 0.0003
AB 0.0000 0.0000 0.9972 0.3512
A2 0.0014 0.0014 44.99 0.0003
B2 0.0004 0.0004 13.20 0.0084
Residual 0.0002 0.0000
Lack of fit 0.0002 0.0001 4.42 0.0925 insignificant
The final Equation in Terms of Actual Factors for all the resposes are presented in Eqn. 1 –
3 for the compressive strength model, weigth loss, and expansion due to sulphate attack. All
the models were quadratic.

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 Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and M. M. A Wahab

𝐶𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ(𝑀𝑃𝑎) = 68.426 + 1.055𝐶𝑅 + 2.974 𝑁𝑆 − 0.222 𝐶𝑅 ∗ 𝑁𝑆 −

0.279 𝐶𝑅 2 − 0.132 𝑁𝑆 2 (1)
𝑊𝑒𝑖𝑔ℎ𝑡 𝑙𝑜𝑠𝑠(%) = 30.933 + 0.877𝐶𝑅 − 1.663 𝑁𝑆 + 0.192 𝐶𝑅 ∗ 𝑁𝑆 − 0.148 𝐶𝑅 2 −
0.388 𝑁𝑆 2 ( 2)
𝐸𝑥𝑝𝑎𝑛𝑠𝑖𝑜𝑛(%) = 0.043 − 0.009 𝐶𝑅 − 0.018 𝑁𝑆 + 0.0005 𝐶𝑅 ∗ 𝑁𝑆 − 0.0027 𝐶𝑅 2 −
0.0023 𝑁𝑆 (3).

a b

c d

e f

Figure 5. RSM response model graphs.

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 Acid and Sulphate Resistance of Nano Silica Rubberized Engineered Cementitious Composite

3.6. Optimization using RSM

The target of optimization is to acquire the best mixtures for the free factors that limit or
augment a specific combination of the independent variables that will give the maximum
compressive strength at minimum weight loss and expansion. Figure 6 demonstrates the best
settings for the investigation with the desirability of 93.7%. The outcomes acquired utilizing
design-expert software were approved tentatively. The factors utilized were crumb rubber and
nano silica as appeared in Table 4. The calculated variations for all the variables were assessed
to discover the legitimacy of the predicted model. The outcomes demonstrate an error of less
than 5% which demonstrates the exactness of the model.

Table 4. Optimization Table

Figure 6. Ramp optimization Models

4. CONCLUSIONS
Based on experimental work and analysis, the following conclusions can be made:
• The propensity of the crumb rubber particles to drive off water and capture air leads to
reduction in strength of the rubberized ECC. The trapped air on the surface of the CR
increases the thickness of the ITZ and causes poor bond with the cement matrix.
• Nano silica could overcome the limitation of rubberized ECC with the right dosage. Several
studies have given positive results in terms of strength, durability and resistance to chemical
attacks for nano silica incorporated rubberized ECC.
• Crumb rubber has also established itself as a viable partial replacement for fine aggregates
in ECC. The pores in the hardened matrix may cause reduction in strength and durability
but it can also be beneficial for the construction industry besides being an eco-friendly
solution for waste tires.

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 Inthiran Mahendran, Bashar S. Mohammed, Sani Haruna and M. M. A Wahab

• Rubberized ECC with nano silica has better chemical attack resistance (acid attack, sulfate
attack and efflorescence) in comparison with normal concrete. The rubberized ECC with
nano silica has the tendency to reduce movement of water transporting the chemicals into
the concrete. Since the rubberized ECC with nano silica has a denser ITZ and porosity, less
chemical can seep into the concrete to deteriorate it.

ACKNOWLEDGEMENT
The authors will like to acknowledge the support and funding for the research under the
Yayasan UTP (YUTP) grant with cost center number: 015LC0-097, Universiti Teknologi
PETRONAS.

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