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Article
Modelling and Optimizing the Durability Performance of Self
Consolidating Concrete Incorporating Crumb Rubber and
Calcium Carbide Residue Using Response
Surface Methodology
Okorie Austine Uche 1 , Sylvia E. Kelechi 1,2 , Musa Adamu 1,3, * , Yasser E. Ibrahim 3, * , Hani Alanazi 4
and Imhade P. Okokpujie 5,6

1 Department of Civil Engineering, Bayero University, P.M.B. 3011, Kano 700006, Nigeria;
uoaustine.civ@buk.edu.ng (O.A.U.); skelechi@pnw.edu (S.E.K.)
2 Department of Mechanical and Civil Engineering, Purdue University, Northwest, Hammond, IN 46323, USA
3 Engineering Management Department, College of Engineering, Prince Sultan University,
Riyadh 11586, Saudi Arabia
4 Department of Civil and Environmental Engineering, College of Engineering, Majmaah University,
Al-Majmaah 11952, Saudi Arabia; hm.alanazi@mu.edu.sa
5 Department of Mechanical and Mechatronics Engineering, Afe Babalola University, Ado Ekiti 360101, Nigeria;
ip.okokpujie@abuad.edu.ng
6 Department of Mechanical and Industrial Engineering Technology, University of Johannesburg,
Johannesburg 2028, South Africa
* Correspondence: madamu.civ@buk.edu.ng (M.A.); ymansour@psu.edu.sa (Y.E.I.)


Citation: Uche, O.A.; Kelechi, S.E.;
Abstract: The world is now focusing on a sustainable environment and reducing the effects of global
Adamu, M.; Ibrahim, Y.E.; Alanazi, warming. One way to achieve such targets is to properly utilize waste and reduce greenhouse CO2
H.; Okokpujie, I.P. Modelling and emissions. The cement industry is responsible for almost 10% of global CO2 emission due to the
Optimizing the Durability high demand for cement in the construction industry. One of the ways to minimize this effect is
Performance of Self Consolidating the partial replacement of cement by other materials in concrete. Therefore, in this study, calcium
Concrete Incorporating Crumb carbide residue (CCR), which is highly rich in calcium oxide, partially replaced cement for waste
Rubber and Calcium Carbide management. Waste tires were grinded to fine sizes in crumb rubber (CR) and partially replaced
Residue Using Response Surface
the fine aggregate. Therefore, this paper investigared the influence of CR and CCR on the durability
Methodology. Buildings 2022, 12, 398.
properties and heat/temperature resistance of self-compacting concrete (SCC). The experiment was
https://doi.org/10.3390/
designed using response surface methodology to investigate the effects of CR and CCR on SCC
buildings12040398
properties, design models for properties of the SCC, and optimize the mixes to achieve the best
Academic Editor: Jorge de Brito results. The properties considered were the durability of acid attack resistance (H2 SO4 attack), salt
Received: 2 February 2022
attack resistance (MgSO4 attack), and water absorption. The heat resistance considered was weight
Accepted: 16 March 2022 reduction and residual compressive strength after heating the samples at a 200 ◦ C and 400 ◦ C. The
Published: 24 March 2022 results findings showed that CR and CCR negatively affect the acid and salt resistance of the SCC.
Furthermore, CR negatively affects the heat resistance of the SCC, while CCR slightly improved
Publisher’s Note: MDPI stays neutral
it at 200 ◦ C. The models developed using RSM were significant with high degrees of correlation
with regard to jurisdictional claims in
and predictability. The optimum properties achieved 2.9% CR as a fine aggregate replacement and
published maps and institutional affil-
iations.
5.5% CCR as a cement replacement. The developed models can predict the durability performance of
SCC mixes in terms of acid and salt attack resistance and the effects of elevated temperatures using
CR, CCR, and fly ash as the variables. This will reduce the need for carrying out experimental work,
thereby reducing cost and time.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland. Keywords: calcium carbide residue; crumb rubber; self-consolidating concrete; response surface
This article is an open access article methodology; elevated temperature; durability
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).

Buildings 2022, 12, 398. https://doi.org/10.3390/buildings12040398 https://www.mdpi.com/journal/buildings


Buildings 2022, 12, 398 2 of 24

1. Introduction
The development of environmentally friendly construction materials has become
the main concern of the building and construction industry’s professionals due to the
global issue of ozone layer depletion caused by greenhouse gases. Cement production
generates substantial by-products that intensify global warming when discharged into
the atmosphere [1]. In order to cut down on the consumption of cement in the building
and construction sector, the partial or full substitution of cement with sustainable and
eco-friendly cementitious materials has to be given serious attention. A study aimed at
promoting the use of local and sustainable construction materials to reduce the impacts
of the continuous use of conventional materials was conducted by Obianyo et al. [2]. On
the other hand, industrial wastes such as used tyres and calcium carbide dumped in the
environment contribute to the significant environmental issues faced by society. Although
efforts have been targeted towards industrial wastes recycling and converting these waste
materials to use raw materials for utilization in diverse industries, the quantity of industrial
wastes abandoned continues to increase due to industrialization [3]. The need to broaden
the utilization of these waste materials has led researchers to identify more applications
areas. The use of calcium carbide residue and crumb rubber from waste tyres by utilizing
them as replacement materials in concrete production is a good idea. Implementing it will
ensure that the consumption of 100% of such industrial waste is generated.
The durability of cement-based materials such as concrete cannot be ignored due to
their heterogeneous nature [4]. The heterogeneity of the concrete matrix results within
the concrete’s microstructure, which significantly affects its durability performance [5]. A
review work conducted by Sofi [6] on the influence of waste rubber tyres on the durability
and mechanical properties of concrete revealed a reduction in the compressive strength,
flexural tensile strength, and depth of water penetration of the rubberized concrete when
compared to the control mix. However, the water absorption (up to 10% replacement) and
abrasion resistance were better than the control mix concrete. Hilal [7] examined the effect of
CR size and content on hardened characteristics of self-compacting concrete and discovered
that the addition of crumb rubber in concrete resulted in a negative effect on the self-
compacting concrete’s hardened properties. However, in terms of ductility, a substantial
improvement was accomplished by adding all types of waste tires. Valizadeh et al. [8]
investigated the influence of specimen geometry on the tensile strengths and compressive
strength of self-compacting rubberized concrete with CR granules. Their findings showed
that the variations between the cubes and cylindrical specimens were higher for the self-
compacting rubberized concrete containing 20% CR in comparison to the mixes with
lower CR content. In addition, a remarkable size effect on the tensile strength of self-
compacting rubberized concrete was observed as the CR aggregate was added. Another
study conducted by Bušić et al. [9] on the mechanical properties of SCC containing recycled
rubber and silica fume indicated that a compressive strength above 30 MPa was obtained
at the optimal combinations with up to 15% of recycled rubber and 5% of silica fume for
28 days curing age According to the authors, this result suggests the possibility of applying
reinforced self-compacting rubberized concrete for structural elements in the future.
Response surface methodology is a design method that generates a set of continu-
ous statistical analysis methods that explores the links between variables and their re-
sponses [10–12]. The major idea of RSM is to determine the relationship between the
dependent and independent variables and study their interactions while obtaining their
optimal responses [13]. The application of RSM in modeling and optimization has been
proven in various fields (e.g., food, electronic technology). Its widespread adoption is
due to its practicality, economy, and relative ease of use [14]. The main advantage of RSM
is that the number of experimental trials required to evaluate multiple parameters and
their interactions is inexpensive [15,16]. RSM is used for two main purposes: modeling
and optimization. The optimization work carried out using RSM covers many research
areas such as waste treatment, the food industry, the welding process, and the sputtering
process [17]. RSM is used for modeling wire discharge machining processes [18], H3 PO4
Buildings 2022, 12, 398 3 of 24

activated rubber waste adsorption in water treatment applications, and wastewater treat-
ment from plants’ palm oil [19]. It is also used in the field (e.g., splatter thin film coating
for electronic Aapplications [20]) and as an additive in concrete for use in the construction
industry [21,22].
RSM has been helpful for modelling and optimization of concrete. Mohammed
et al. [23] employed RSM to develop a model that predicts paper mill concrete’s compressive
strength. Haruna et al. [24] also utilized RSM to predict the compressive strength of
mortar by developing an optimization model. Rezaifar et al. [25] developed a model
and optimized high-performance concrete using metakaolin and fly ash as variables to
minimize the durability coefficient and maximize compressive strength. Mohammed
et al. [26] developed a model to predict compressive strength, unit weight, and water
absorption of rubber created using RSM. They also optimized the rubber to create a mix by
maximizing compressive strength and minimizing water absorption. Alyamac et al. [27]
developed a self-compressing engineering cement composite (SC-ECC) mixed design
model using RSM. They also optimize the ECC blend by maximizing elasticity and energy
absorption. Vincent [28] examined the properties of rubberized concrete containing waste
tire steel reinforcement at an early age. They analyzed the compressive strength, splitting
tensile strength, and flexural strength using RSM. The normal residual plots indicated that
the model was very appropriate. Haruna et al. [10] used RSM to investigate the effect of
NaOH on the molarity of outdoor cured geopolymer mortars containing high calcium fly
ash. They further conducted optimization and discovered the best mix contains 10Molarity
Sodium hydroxide concentration and 0.5 water binder ratio, which yielded maximum
compressive strength and flowability within range.
Several researchers reported that CR has many advantages when used in concrete,
such as improved ductility, energy absorption capacity, thermal insulation, etc. [12,29,30].
However, the major drawback in using CR in concrete is its negative effect on concrete’s
mechanical and durability performance. Many methods of mitigating the negative effect
of CR on concrete have been carried out. However, there are limited studies that utilize
the hybrid of fly ash and CCR as cementitious materials to mitigate the negative effect
of CR on the durability performance of SCC. Although the combination of CCR and fly
ash is expected to significantly enhance the durability of SCC due to the reaction between
SiO2 from fly ash, Ca(OH)2 can be used from CCR to generate secondary C-S-H gels.
These C-S-H gels are expected to fill the pores created by the CR in the cement matrix and
densify the concrete’s microstructure, enhancing strength and durability. Studies in the
application of RSM modelling in durability performance prediction of green SCC utilizing
CR as a partial substitute to fine aggregate and CCR as cement replacement material are
limited. Therefore, there is a need for more research in using RSM analysis in predicting
the durability performance of various green concretes such as SCC. Therefore, in this
study, RSM was used for designing the experiments developing models to predict the
durability performance and elevated temperature resistance of SCC using CR and CCR as
the variables.

2. Materials and Methods


2.1. Materials
This research utilized type 1 ordinary Portland cement of 3.5 specific gravity in con-
formity with the BS EN 196-6 [27] specification as the principal binding substance. The
XRF result showing the chemical composition of cement is presented in Table 1. The fly ash
employed as supplementary cementitious material for this study belongs to class F under
ASTM C618 [28], as shown in Table 1. The CCR samples were obtained from an industrial
welding shop depot. The CCR sample was initially dried in the air for four days, and to
ensure it was completely dried, and it was further dried in the oven for 24 h at 110 ± 5 ◦ C
temperature. The CCR was grinded and sieved through sieve No. 325 (45 µm) to obtain a
smooth powder. The particles that passed the sieve were utilized for this experiment, and
the retained ones in the sieve were trashed. The properties of CCR were also obtained using
to obtain a smooth powder. The particles that passed the sieve were utilized for this
Buildings 2022, 12, 398
experiment, and the retained ones in the sieve were trashed. The properties of CCR4were of 24

also obtained using XRF and shown in Table 1. Its microstructural morphology as ob-
tained through scanning electron microscopy is presented in Figure 1. The joint particle
XRF
size and shown inplot
distribution Table 1. Itsaggregate,
of Fine microstructural
coarsemorphology
aggregate, andas obtained
CR shown through scanning
in Figure 2 was
electron
used formicroscopy
the study. Inis presented
accordance inwith
Figure 1. The
[29], jointfine
CR and particle size distribution
aggregate both belong plot
to of FineII
zone
aggregate, coarse particle
class and exhibit aggregate, and
size. The CRfine
shown in Figure
aggregate was2natural
was used forsand
river the study.
with aInspecific
accor-
dance
gravity with [29], water
of 2.63, CR andabsorption
fine aggregate both belong
of 1.96%, to zoneofII1560
bulk density classkg/m
and exhibit particle
3, and mud size.
content
The fine aggregate was natural river sand with a specific gravity of 2.63,
of 1.1%. The CR had a specific gravity of 0.95. The coarse aggregate consists of 19mm water absorption
of 1.96%, bulk density of gravel
1560 kg/m 3, and mud content of 1.1%. The CR had a specific
maximum-sized crushed with specific gravity, bulk density, and water absorption
gravity
of 2.65, of 0.95.
1450 The3, coarse
kg/m aggregate
and 0.94%, consists Also,
respectively. of 19mm maximum-sized
self-compaction of thecrushed
concrete gravel
was
with specific gravity, bulk density, 3, and 0.94%,
achieved with the incorporation ofand water absorption
a superplasticizer. Theofsuperplasticizer
2.65, 1450 kg/mbelongs to the
respectively. Also, self-compaction
polycarboxylate-based classificationof the
withconcrete was achieved
a density with and
of 1.11 kg/L the incorporation
dosage of 2 of to
a15bfl.oz/cwt
superplasticizer. The superplasticizer
of cementitious materials. belongs to the polycarboxylate-based classification
with a density of 1.11 kg/L and dosage of 2 to 15 bfl.oz/cwt of cementitious materials.
Table 1. Properties of binder materials.
Table 1. Properties of binder materials.
Oxide Composition Cement CCR
Oxide Composition
SiO2 Cement 12.00 CCR 1.1
SiO2 Al2O3 12.00 3.01 1.1 0.04
Al2 O3 Fe2O3 3.01 4.11 0.04 0.5
Fe2 O3 4.11 0.5
CaO
CaO 74.03
74.03 96.46
96.46
MgO MgO 1.3 1.3 0 0
SO3 SO3 2.07 2.07 0.29 0.29
Na2 O Na2O 0.19 0.19 0.01 0.01
K2 O 1.28 0.45
K 2O 1.28 0.45
LOI 1.02 1.02
Specific GravityLOI 3.15 1.02 2.22 1.02
Specific Gravity 3.15 2.22

Figure 1.
Figure 1. Microstructural
Microstructural morphology
morphologyof
ofCCR.
CCR.

Buildings 2022, 12, x. https://doi.org/10.3390/xxxxx www.mdpi.com/journal/buildings


Buildings 2022,
Buildings 2022, 12,
12, 398
x 2 5of
of 16
24

sand BS 882 zone 2 upper limit BS 882 Zone 2 lower limit


coarse aggregate CR
100
90
80
70
Passing (%)

60
50
40
30
20
10
0
0 0 1 10 100
Sieve Size (mm)

Figure
Figure 2.
2. Aggregates
Aggregates gradation.
gradation.

Experimental Design Using RSM


2.2. Experimental
Response surface methodology
Response methodology (RSM) gathers arithmetical
arithmetical and analytical methods
for computing
computing the correlation among a class of independent measurable variables with
one or
one or more
more responses
responses [31,32].
[31,32]. RSM
RSM can
can be
be utilized
utilized to
to find
find functioning
functioning variables
variables that
that may
may
significantly affect the basic response or not [33]. RSM could also be defined as
significantly affect the basic response or not [33]. RSM could also be defined as a cornuco- a cornucopia
of arithmetical
pia andand
of arithmetical analytical methods
analytical methodsfor for
modeling
modeling andand analyzing
analyzingproblems.
problems.The output
The out-
is determinant
put by numerous
is determinant by numerous factors (input
factors variables)
(input [27]. RSM
variables) [27]. is
RSMalsoisbeneficial for multi-
also beneficial for
faceted models by establishing preferable goals in terms of response or
multi-faceted models by establishing preferable goals in terms of response or variablesvariables [26]. RSM
analysis
[26]. RSMcan be achieved
analysis with various
can be achieved withdesign
variousmodels,
design including central composite,
models, including Box-
central compo-
Behnken, and historical data. These can be used to generate the arithmetical
site, Box-Behnken, and historical data. These can be used to generate the arithmetical cor- correlation
responseresponse
relation and independent variables.variables.
and independent The number The of variables
number and each and
of variables variable
eachvariation
variable
is key determinants for the design model type [34]. The first-order function
variation is key determinants for the design model type [34]. The first-order function gives the linear
gives
model as shown in Equation (1).
the linear model as shown in Equation (1).
𝑦=
y= β 0𝛽+ +
β 1𝛽X1𝑋++β𝛽
2 X𝑋
2++....... +
. . . β. 𝛽
n X𝑋n +
+ξ𝜉 (1)
where
where yy is
is the
the modeled
modeledresponse,
response,ββ00isisthe
they-intercept
y-interceptfor
forwhich
whichXX 1 = X2 = 0, β1, and β2 are
1 = X2 = 0, β1, and β2 are
the coefficients of the first and second independent variables, respectively,
the coefficients of the first and second independent variables, respectively, X X11 is
is the
the first
first
variable coefficient,XX22isisthe
variable coefficient, thesecond
secondvariable
variablecoefficient,
coefficient, and
and ξ isξ the
is the error.
error. Nevertheless,
Nevertheless, the
the linear
linear modelmodel doesn’t
doesn’t matchmatch
the the data’s
data’s response
response whenwhen curvature.
curvature. A second-order
A second-order func-
function
tion
with with a higher
a higher degreedegree polynomial
polynomial modelmodel
will bewill be utilized,
utilized, as shown as shown in Equation
in Equation (2) [11]. (2)
[11].
k k
y = β 0 + ∑ β i Xi + ∑ β ii Xi2 + ∑ ∑ β ij Xi X j + ξ (2)
𝑦 = 𝛽 +i=1 𝛽 𝑋 +i=1 𝛽 𝑋 +i<1 j 𝛽 𝑋 𝑋 + 𝜉 (2)

The CCD has a factor planning component of 2k, where k is the number of related
The CCD has a factor planning component of 2k, where k is the number of related
variables or factors operated at two levels of a low and high number [24]. The variable
variables or factors operated at two levels of a low and high number [24]. The variable
lower and upper limits are coded with negative and positive numbers, respectively. The
lower and upper limits are coded with negative and positive numbers, respectively. The
central point of the central composite design is the average of upper and lower limits from
central point of the central composite design is the average of upper and lower limits from
the factorial design [35]. Hence the center point is described as the zero-point area that
the factorial
meets designconditions.
the optimal [35]. Hence the center point is described as the zero-point area that
meets the optimal conditions.
Buildings 2022, 12, 398 6 of 24

The experiment was designed and statistically analyzed using RSM from design
expert version 10 software in this study. The mathematic models between variables and
response were developed. Modelling of a variable using response surface methodology
(RSM) involves a sequence of processes to achieve the research objective, which requires
recognizing the research problem based on the formulated research optimization goals.
In this study, the face-centered central composite design (FCCCD) available in the RSM
software having α = 1 was used to develop mathematical models to predict the relationships
between the variables and responses. The independent variables considered were CR as
partial replacement to fine aggregate, which varied at three levels (i.e., 0%, 10%, and 20%) by
volume of sand. The second variable was CCR as partial replacement to cement and varied
into three levels (i.e., 0%, 5%, and 20%) by volume of cement. The responses were weight
reductions due to immersion in acidic (H2 SO4 ) and salt (MgSO4 ), and water absorption.
Other responses were residual compressive strength and weight reductions due to elevated
temperatures (normal temperature, 200 ◦ C, and 400 ◦ C). The RSM software-generated
thirteen (13) mixes with regards to the various combinations of the variables, as shown in
Table 2. From Table 2, the water-to-binder ratio (W/B) was not constant (unified). This
is due to the fact that the CCR was used as a partial replacement by volume of cement
and not by weight. Due to the lower specific gravity of the CCR compared to cement, this
resulted in variation in total weight of the cementitious materials, resulting in variation of
the W/B ratio across the mixes.

Table 2. Experimental design mix and constituent materials.

Factors Constituent Materials for 1 kg/m3

Run/Mix Fine Coarse


A: CR B: CCR Cement CCR CR Water SP
Agg Agg W/B
(%) (%) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 )
(kg/m3 ) (kg/m3 )
1 0 0 520 0 880 0 850 192.4 7.80 0.37
2 0 10 468 36.65 880 0 850 192.4 7.59 0.38
3 10 5 494 18.32 792 38.25 850 192.4 7.68 0.38
4 10 5 494 18.32 792 38.25 850 192.4 7.68 0.38
5 10 10 468 36.65 792 38.25 850 192.4 7.59 0.38
6 20 10 468 36.65 704 76.49 850 192.4 7.59 0.38
7 10 5 494 18.32 792 38.25 850 192.4 7.68 0.38
8 20 5 494 18.32 704 76.49 850 192.4 7.68 0.38
9 10 5 494 18.32 792 38.25 850 192.4 7.68 0.38
10 10 0 520 0 792 38.25 850 192.4 7.80 0.37
11 20 0 520 0 704 76.49 850 192.4 7.80 0.37
12 0 5 494 18.32 880 0.00 850 192.4 7.68 0.38
13 10 5 494 18.32 792 38.25 850 192.4 7.68 0.38
A = CR, crumb rubber; B = CCR, calcium carbide residue; W/B: water-to-binder ratio.

2.3. Samples Preparation and Test Methods


BS 1881-125 [36] specifications were used for batching, sampling, and mixing the fresh
concrete. The mixing of the fresh concrete was carried out with the aid of a rotating pan
mixer in the Laboratory at room temperature and relative humidity. The fresh concrete was
cast into the specified moulds, followed by immediately mixing and allowed to harden for
one day. After that, they were demoulded and cured in water for the stated duration before
the evaluation.
The durability test was conducted with resepct to acid attack, salt attack, and water
absorption. Guidelines outlined in ASTM C642 [37] were used to measure the resilience of
the SCC samples to acid and salt attacks. After curing in water for 28 days, the 100 mm
cubes were immersed in H2 SO4 and MgSO4 solutions for 28 days to measure resistance to
acid and salt, respectively. Prior to immersion in the solutions, the samples were weighed.
After 28 days period of immersion, the samples were reweighed and recorded. Three
samples were tested for the acid and salt attacks and the average value recorded for each
Buildings 2022, 12, 398 7 of 24

mixture. For the effect of elevated temperatures on the SCC mixes, 28 days of water curing
was conducted on the 100 mm cube samples before testing. After curing, the samples
were air-dried and weighed before subjecting to elevated temperature. The samples were
then exposed to heat for 1 h at different temperatures of 200 ◦ C and 400 ◦ C, respectively.
The specimens were air-cooled and weighed after that. The samples were then tested for
compressive strength in accordance with BS EN 12390-3 [38] specification. The weight
reduction was then calculated using Equation (3). Triplicate samples were tested for all
of the mixtures and elevated temperature and mean value were recorded. The water
absorption test was carried out using 100 mm cube samples in accordance with ASTM
C642 [37] specifications. The specimens were water cured for 28 days prior to water
absorption determination. Three samples were tested for water absorption and the mean
value was also recorded.
W
WR (%) = i × 100 (3)
Wn
where WR represents the weight reduction in %, Wi and Wn represent the initial and final
weights respectively in kg.

3. Results and Discussions


3.1. Durability Performance against Acid and Salt Attack
Statistical models have been generated using RSM to speculate the acid and salt attack
resistance of the SCC mixes containing CR and CCR. The acid attack was measured by
immersing the samples in H2 SO4 solution for 28 days, and then the weight reduction was
calculated. Similarly, the salt attack was measured by immersing the samples in magnesium
sulphate (MgSO4 ) solution for 28 days, and then weight reduction was computed. The
results are presented in Table 3.

Table 3. Results of durability test on SCC mixes.

Factors (%) Responses


Run/Mix Weight Reduction in H2 SO4 (%) Weight Reduction in MgSO4 (%) Water
A: CR B: CCR Absorption
3 Days 7 Days 28 Days 3 Days 7 Days 28 Days
(%)
1 0 10 2.83 4.39 7.78 0.5 1.25 1.89 1.74
2 0 0 3.81 5.87 10.17 0.83 1.63 2.78 1.74
3 10 5 2.26 3.29 4.24 0.31 0.78 1.14 2.35
4 10 5 2.35 3.13 4.67 0.32 0.78 1.13 2.26
5 10 10 1.65 3.27 4.12 0.3 0.57 0.99 2.5
6 20 10 1.8 3.5 5.45 0.5 1.2 1.5 2.15
7 10 5 2.14 3.33 4.41 0.34 0.77 1.11 2.19
8 20 5 2.2 4.27 6.00 0.86 1.5 2.2 2.19
9 10 5 2.25 3.42 3.96 0.29 0.72 1.25 2.39
10 10 0 2.71 3.82 6.58 0.42 1.15 2.04 2.37
11 20 0 4 5.95 10.4 0.9 1.68 2.91 2.83
12 0 5 3.3 5.8 9.49 0.53 1.54 2.16 1.76
13 10 5 2.08 3.28 3.67 0.43 0.86 1.05 2.26

The RSM developed models to predict the weight reductions of the SCC in H2 SO4 and
MgSO4 solutions using CR and CCR as the variables. Furthermore, the water absorption
of the SCC mixes was also modelled statistically. The developed models were explained
statistically using analysis of variance (ANOVA), as presented in Table 4. The probability
(P-Significance) test was used to explain the significance of the models and each model
term. A model or its term has been said to be significant if its p-value is less than 0.05,
implying that the null hypothesis has been proven to be statistically true. The lower the
p-values, the higher the agreement of the null hypothesis with the corresponding developed
models and vice versa. From Table 4, the models for predicting the weight reduction due
to immersions in H2 SO4 and MgSO4 and water absorption were all statistically significant
Buildings 2022, 12, 398 8 of 24

with p-values far less than 0.05. the F-values of 30.16, 81.04, and 11.21 for weight reduction
(H2 SO4 ), weight reduction (MgSO4 ), and water absorption models, respectively, indicated
that they were all significant against their corresponding null hypotheses. The significance
of each of the model terms can also be explained using p < 0.05. For weight reduction due
to immersion in the H2 SO4 model, the model terms CR, CCR, and (CR)2 were statistically
significant in the model with p values below 0.05. At the same time, interaction between
CR and CCR (i.e., CR ∗ CCR and (CCR)2 ) were not significant as their p values are greater
than 0.05. For weight reduction due to immersion in the MgSO4 model, the terms CCR,
(CR)2, and (CCR)2 were statistically significant, while the terms CR and CR*CCR were
not significant statistically. Additionally, for the water absorption model, the terms CR,
CR ∗ CCR, and (CR)2 were all statistically significant within the model, while the terms
CCR and (CCR)2 were not statistically significant.

Table 4. ANOVA for durability responses models.

Sum of Mean F p-Value


Responses Source Significance
Squares Square Value Prob > F
Model 69.37 13.87 30.16 0.0001 significant
A-CR 5.21 5.21 11.32 0.0120 significant
B-CCR 16.01 16.01 34.80 0.0006 significant
28 Days- AB 1.64 1.64 3.56 0.1011 not significant
Immersion in A2 30.72 30.72 66.79 <0.0001 significant
H2 SO4 B2 2.44 2.44 5.31 0.0547 not significant
Residual 3.22 0.46 - - -
Lack of Fit 2.62 0.87 5.77 0.0618 not significant
Pure Error 0.60 0.15 - - -
Model 5.31 1.06 81.04 <0.0001 significant
A-CR 0.008067 0.008067 0.62 0.4583 not significant
B-CCR 1.87 1.87 142.80 <0.0001 significant
28 Days- AB 0.068 0.068 5.16 0.0573 not significant
Immersion in A2 2.26 2.26 172.50 <0.0001 significant
MgSO4 B2 0.16 0.16 12.09 0.0103 significant
Residual 0.092 0.013 - - -
Lack of Fit 0.071 0.024 4.46 0.0915 not significant
Pure Error 0.021 0.00528 - - -
Model 1.07 0.21 11.21 0.0031 significant
A-CR 0.62 0.62 32.63 0.0007 significant
B-CCR 0.050 0.050 2.65 0.1476 not significant
AB 0.12 0.12 6.08 0.0432 significant
Water
A2 0.28 0.28 14.63 0.0065 significant
Absorption (%)
B2 0.056 0.056 2.95 0.1295 not significant
Residual 0.13 0.019 - - -
Lack of Fit 0.11 0.036 5.66 0.0637 not significant
Pure Error 0.025 0.0063 - - -

The statistical lack of fit, which is defined as the amount, the model predictions missed
the observations, was further used to evaluate each model’s significance. The F values of
5.77, 4.46, and 5.66 for weight reduction (H2 SO4 ), weight reduction (MgSO4 ), and water
absorption models, respectively. It implied only 6.18%, 9.15%, and 6.37% probabilities
for weight reduction (H2 SO4 and weight reduction (MgSO4 ). Also, the water absorption
models, respectively, indicated that the lack of fit for those F-values could arise due to noise.
For the model to be fit, its lack of fit should be non-significant [11,32,39]. For the weight
reduction (H2 SO4 ), weight reduction (MgSO4 ), and water absorption model, their p-values
for the lack of fits were greater than 0.05. Therefore, all of the models were said to fit
well. Their lack of fit was not significantly relative to their corresponding pure errors. The
Buildings 2022, 12, 398 9 of 24

developed statistical models for the weight reduction (H2 SO4 ), weight reduction (MgSO4 ),
and water absorption models are presented as Equations (4)–(6), respectively.

WR (H2 SO4 ) = 10.453 − 0.696 × A − 0.575 × B − 0.0128 × A × B


(4)
+0.0334 × A2 + 0.0376 × B2

WR(MgSO4 ) = 2.785 − 0.172 × A − 0.181 × B − 0.0026 × A × B


(5)
+0.009 × A2 + 0.0096 × B2
W.A (%) = 1.716 − 0.113 × A − 0.041 × B − 0.0034 × A × B + 0.0032 × A2
(6)
+0.0057 × B2
where WR represents weight reduction in %, W.A represents water absorption in %, A
represents crumb rubber (CR) in %, and B represents calcium carbide residue (CCR) in %.
The degree of quality, adequacy, fitness, and predictability of the durability models
was further investigated and explained using the ANOVA (i.e., degree of determination
(correlation)), as given in Table 5. An R2 value of 1 (unity) implied a perfectly fitted model,
while a lower R2 value implied a poorly fitted model. All of the generated prototypes
have more significant degree of correlations (R2 ≥ 0.9), which implies that for all of the
models, only less than 10% of the experimental data could not be explained by the models.
The R2 values of 0.956, 0.983, and 0.90 for the weight reduction (H2 SO4 ), weight reduction
(MgSO4 ), and water absorption models, respectively, implied that all of the experimental
data were fitted and explained by the model except 4.4%, 1.7%, and 10% for the weight
reduction (H2 SO4 ), weight reduction (MgSO4 ) and water absorption models, respectively.
The model’s adequacy and fitness were further evaluated using the difference between
the predicted and adjusted R2 values. For a model to be fit, the speculated and adjusted
R2 values need to be reasonably in consensus to each other (i.e., their differences should
be less than 0.2). For the weight reduction (MgSO4 ) model, its predicted and adjusted R2
agreed as their differences are less than 0.2. However, for weight reduction (H2 SO4 ) and
water absorption models, the difference between their predicted and adjusted R2 values
was greater than 0.2. This might be due to a problem with the model or data or might
indicate a large block effect. Therefore, model reduction through backward elimination
was carried out to remove the non-significant model terms. The coefficient of variations
(CoV) was similarly employed to determine the dispersion of test information across the
predicted prototypes. From Table 5, the water absorption model had the least CoV value of
6.24%. In comparison, the weight reduction (H2 SO4 ) immersion had the highest CoV value
of 10.89%. All of the models can be said to be a lower CoV value and can therefore be used
to predict the responses with a lower residual error related to its predicted values. The
signal to noise levels for each model was measured using adequate precision. Every single
one of the prototypes recorded an adequate precision value greater than foru, meaning
that the prototype can be applied to cruise the design domain as defined by the model
type selected.
The degree of determination (correlation) for the weight reduction (H2 SO4 ) and water
absorption models after removing the non-significant model terms through backward
elimination are given in Table 5. It can be observed that after model reduction, the predicted
and adjusted R2 values for both the weight reduction (H2 SO4 ), and water absorption were
now following one another as their differences were below 0.2. The developed mathematical
models after the non-significant terms were removed for the weight reduction (H2 SO4 ) and
water absorption models are presented as Equations (7) and (8), respectively. The backward
elimination for the models reduction was selected algorithmically by the RSM software
using, multiple model selection methods and criteria. The best one-term-smaller model
(insignificant term) for the selected criteria was kept in order to improve the criterion score
as in Equation (8) where the model insignificant term B representing CCR was kept. If the
best one-term does not improve the cretarion score, then the whole insignifant terms were
removed as in Equation (7) [40].
Buildings 2022, 12, 398 10 of 24

Table 5. Coefficient of determination for durability models.

Before Model Reductions After Model Reduction

Factors Weight Weight Water Absorption Weight Water


Reduction-H2 SO4 Reduction-MgSO4 (%) Reduction-H2 SO4 Absorption (%)
Immersion (%) Immersion (%) Immersion (%)
Std. Dev. 0.68 0.11 0.14 0.90 0.15
Mean 6.23 1.70 2.21 6.23 2.21
C.V. % 10.89 6.72 6.24 14.47 6.96
PRESS 27.03 0.56 1.13 19.84 1.00
R2 0.956 0.983 0.900 0.8994 0.8422
Adjusted R2 0.924 0.971 0.810 0.8659 0.7633
Predicted R2 0.628 0.897 0.355 0.7267 0.5676
Adequate Precision 14.961 27.20 11.18 15.797 10.307

WR (H2 SO4 ) = 10.78 − 0.832 × A − 0.327 × B + 0.0369 × A2 (7)


WA(%) = 1.668 + 0.102 × A − 0.016 × B − 0.0034 × A × B + 0.0026 × A2 (8)
where WR represents weight reduction in %, WA represents water absorption in %, A
represents crumb rubber (CR) in %, and B represents calcium carbide residue (CCR) in %.
Based on the RSM analysis, the difference between the predicted and adjusted R2
values must be less than 0.2. If their difference is greater than 0.2, this might indicate
a large block effect or possible problem with the model or data. Therefore, to fix this
error, model reduction by removing the insignificant terms in the model is required [39,40].
Equations (7) and (8) are the statistically modified versions of Equations (4) and (6), re-
spectively which were obtained after model reduction through backward elimination by
removing the insignificant model terms. As seen in Table 5, after the model reductions, the
models’ predicted, and adjusted R2 values will be reasonably in agreement with each other.
Therefore, Equations (7) and (8) are the statistically fitted models for predicting the weight
reductions due to H2 SO4 emissions and water absorption, respectively, for the SCC mixes
containing CR and CCR.
The models’ adequacy and degree of correlation for predicting the durability of SCC
mixes were checked and verified graphically by plotting the normal plots against internally
studentized residuals. From the normal plots against internally studentized residuals as
presented in Figure 3, all of the models followed the normal probability distribution. They
were all set on the straight line. Hence, the normal probability distribution assumed and
used for the statistical models is true. Additionally, all of the data points were reasonably
aligned across the linear trend line. This further explained all of the models’ high R2 values,
greater than or equal to 0.9. Consequently, the initiated models can speculate the weight
reductions due to immersion in H2 SO4 and MgSO4 and water absorption of the SCC mixes
using CR and CCR as the variables with the opulence of accuracy and likelihood.
Figure 4 presents the 3D response surface plots for the for-weight reduction (H2 SO4 ),
weight reduction (MgSO4 ), and water absorption models, respectively. From Figure 4a,b,
the weight reduction due to immersion in H2 SO4 for the SCC mixes was shown to decrease
with the incorporation of 10% CR and then increase with a higher amount of CR up to 20%.
From the 3D plot, the bluish portion, which indicated the lowest weight reduction due
to H2 SO4 immersion, was obtained at the 10% CR coordinate point. The highest weight
reduction was obtained at the 20% coordinate point. Therefore, the partial replacement of
up to 10% fine aggregate with CR increases the acid and salt attack resistance of the SCC.
This improvement in acid and salt resistance of the SCC due to the incorporation of CR
can be attributed to the fact that rubber particles acted as confinement to other particles
such as the cementitious matrix and protected them from separation [41]. Another reason
might be attributed to the bridging provided by the CR due to its higher elasticity and fiber
nature. Resulting in the prevention of crack development caused by the internal pressure
caused by the acid reaction within the concrete microstrip, thereby preventing spalling [42].
Similar findings have been reported by Thomas et al. [41] and Bisht and Ramana [43]. The
increase in weight reduction due to H2 SO4 and MgSO4 CR immersion can be traced to the
The models’ adequacy and degree of correlation for predicting the durability of SCC
mixes were checked and verified graphically by plotting the normal plots against inter-
nally studentized residuals. From the normal plots against internally studentized residu-
als as presented in Figure 3, all of the models followed the normal probability distribution.
They were all set on the straight line. Hence, the normal probability distribution assumed
Buildings 2022, 12, 398 11 of 24
and used for the statistical models is true. Additionally, all of the data points were reason-
ably aligned across the linear trend line. This further explained all of the models’ high R2
values, greater than or equal to 0.9. Consequently, the initiated models can speculate the
increased voids initiated
weight reductions due toby the CR in in
immersion theHcement pattern
2SO4 and MgSOdue
4 andto water
air entrainment
absorptionduring
of the
mixing.
SCC mixesThese voids
using CRinand
theCCR
strongascement patternwith
the variables expand easily in the
the opulence acidic environment
of accuracy and likeli-
causing
hood. deterioration of the cement paste and higher weight reduction [44].

(a) (b)

(c)
Figure 3.
Figure 3. Normal plotsplots against
against internally
internallystudentized
studentizedresiduals
residualsfor
fordurability
durabilitymodels.
models.(a)(a)
Weight
Weight
Loss (H
Loss SO44),), (b)
(H22SO (b) Weight Loss (MgSO
Weight Loss (MgSO44),), and
and (c)
(c) Water Absorption.
Water Absorption.
Buildings 2022,
Buildings 12, x398
2022, 12, 1012of
of 16
24

(a) (b)

(c)
Figure
Figure 4.
4. 3D
3D Response
Response surface
surface plot
plot for
for durability
durability properties
properties for
for (a)
(a) Weight Loss (H
Weight Loss (H2SO 4), (b) Weight
2 SO4 ), (b) Weight
Loss (MgSO 4), and (c) Water Absorption.
Loss (MgSO4 ), and (c) Water Absorption.

3.2. Elevated Temperature


Additionally, the decrease in salt resistance due to CR was due to the high pores in the
hardened cement matrix
The heat resistance of resulting
the SCC from the aircontaining
samples entrapped CRon the
andsurface
CCR wasof the CR during
measured in
mixing. This
residual increased
compressive the internal
strength pressure
and weight on the cement
reduction matrix bythe
after subjecting theconcrete
sulfate-related
to dif-
growthtemperature
ferent crystals, causing internal
exposures. Thecracks andare
results hence deterioration
presented in Tableof6.the cement
RSM pasteused
was then [44,45].
to
Furthermore,
develop models a large amount
to predict the of crystals
residual produced in
compressive the pores
strength andof the matrix
weight by the
reduction of salt
the
solution
SCC causes
mixes large crystallization
at different temperatures. pressure causing deterioration of the cementitious
matrix [46]. Incorporating CCR into the SCC mixes slightly decreases its weight reduction
due to immersion in H2 SO4 and MgSO4 , as shown in Figure 4a,b, respectively. This
implied that CCR slightly increases the resistance of the SCC mixes to acid and salt attacks.
This improvement was more pronounced on the SCC mixes containing 10% CR as partial
replacements to fine aggregate. The reduction in acid and salt might be attributed to the high
Buildings 2022, 12, 398 13 of 24

quantity of CaO in CCR, which reacts with the cement’s chemical oxides. Thus increasing
pozzolanic reaction, densifying the concrete’s microstructure, and reducing ingress of
acids and salts [47]. Regarding the water absorption, from Figure 4c, there is a significant
increment in water absorption with an increase in CR content. This was attributed to the
increment in the pores in the hardened cement paste caused by the hydrophobic nature of
the CR. The CR captures air during mixing causing high porosity when the sample cubes
have dried fully. This leads to an increment in water absorption [11,44,48]. The addition of
CCR slightly decreased the water absorption of the SCC mixes. This might be due to the
filling effect of the CCR, which makes it fill the pores in the SCC mix and hence reduces
water absorption [44,49].

3.2. Elevated Temperature


The heat resistance of the SCC samples containing CR and CCR was measured in
residual compressive strength and weight reduction after subjecting the concrete to different
temperature exposures. The results are presented in Table 6. RSM was then used to develop
models to predict the residual compressive strength and weight reduction of the SCC mixes
at different temperatures.

Table 6. Results for elevated temperatures of SCC mixes.

Factors (%) Residual Compressive Strength Weight Reduction (%)


Run/Mix
R: CR C: CCR 27 ◦ C 200 ◦ C 400 ◦ C 200 ◦ C 400 ◦ C
1 0 10 38.6 38.9 33.8 0.37 3.89
2 0 0 43.5 38.6 34.1 0.39 3.11
3 10 5 41.4 37.7 30.4 0.45 4.1
4 10 5 42.5 39.27 27.2 0.53 4.74
5 10 10 36.2 37.8 29.5 0.44 4.61
6 20 10 32.5 35.4 27 1.4 5.39
7 10 5 39.6 35.75 31.17 0.37 3.76
8 20 5 34.2 35.2 27.6 1.42 5.38
9 10 5 40.26 38.8 29.63 0.41 3.97
10 10 0 37.12 37.6 31 0.46 4
11 20 0 35.6 35 28 1.43 5.35
12 0 5 45.2 38.8 34 0.38 3.75
13 10 5 43.11 38.5 27.87 0.36 4.32

3.2.1. Residual Compressive Strength


RSM has been used to develop models to predict the residual compressive strengths of
the SCC mixes at normal temperature (27 ◦ C) and elevated temperatures of 200 ◦ C and 400
◦ C using CR and CCR as the variables. The ANOVA summary of the developed models

is presented in Table 7. Using the P-Significance test, all of the models for the residual
compressive strength were statistically significant, with p-values less than 0.05. Therefore,
the null hypothesis for all of the models was proven to be true. The models F-values of 10.43,
4.01, and 7.85 for residual compressive strengths at 27◦ C, 200 ◦ C, and 400 ◦ C, respectively,
indicated that they were all significant against their corresponding null hypotheses. The
significance of each of the model terms can also be explained using p < 0.05. For residual
compressive strength at the 27 ◦ C model, the model terms CR and (CCR)2 were statistically
significant with p values less than 0.05. All other terms were not significant as their p values
were greater than 0.05. For residual compressive strengths at 200 ◦ C and 400 ◦ C models,
only the model term CR is statistically significant. Still, all other model terms were not
significant statistically. All of the model’s lack fit was not significant as their p-values were
greater than 0.05. The F values of 2.00, 0.011, and 0.12 for residual compressive strengths
at 27 ◦ C, 200 ◦ C, and 400 ◦ C models, respectively, implied that there is 25.59%, 99.82%,
and 94.22%. The probabilities for residual compressive strengths at 27 ◦ C, 200 ◦ C, and
400 ◦ C models, respectively. Tthat the lack of fit those F-values could arise due to noise.
For the model to be fit, its Lack of fit should be non-significant [11,32,39]. Therefore, all
Buildings 2022, 12, 398 14 of 24

of the models were said to fit well. Their lack of fit was not significant relative to their
corresponding pure errors. The developed statistical models for the residual compressive
strengths at 27 ◦ C, 200 ◦ C, and 400 ◦ C are presented as Equation (9a–9c), respectively.

FC,R (27 ◦ C) = 43.211 − 0.374 × A + 1.003 × B + 0.009 × A × B − 0.0044 × A2 − 0.139 × B2 (9a)

FC,R (200 ◦ C) = 38.585 − 0.007 × A + 0.0927 × B + 0.0005 × A × B − 0.007 × A2 − 0.0067 × B2 (9b)

FC,R (400 ◦ C) = 34.418 − 0.51 × A + 0.25 × B + 0.0035 × A × B − 0.01 × A2 − 0.0192 × B2 (9c)


where FC,R represents the residual compressive strength in MPa, A represents CR in %, and
B represents CCR in %.

Table 7. ANOVA for elevated temperature models for SCC mixes.

Sum of Mean F p-Value


Response Source
Squares Square Value Prob > F
Model 161.63 32.33 10.43 0.0038 significant
A-CR 104.17 104.17 33.60 0.0007 significant
B-CCR 13.26 13.26 4.28 0.0774 not significant
Residual
AB 0.81 0.81 0.26 0.6250 not significant
Compressive
A2 0.53 0.53 0.17 0.6928 not significant
Strength (27 ◦ C)
B2 33.37 33.37 10.77 0.0135 significant
(MPa)
Residual 21.70 3.10 - - -
Lack of Fit 13.03 4.34 2.00 0.2559 not significant
Pure Error 8.67 2.17 - - -
Model 22.12 4.42 4.01 0.0488 significant
A-CR 19.08 19.08 17.31 0.0042 significant
B-CCR 0.14 0.14 0.12 0.7367 not significant
Residual
AB 0.0025 0.0025 0.00227 0.9633 not significant
Compressive
A2 2.09 2.09 1.89 0.2113 not significant
Strength
B2 0.079 0.079 0.072 0.7964 not significant
(200 ◦ C) (MPa)
Residual 7.72 1.10 - - -
Lack of Fit 0.062 0.021 0.011 0.9982 not significant
Pure Error 7.66 1.91 - - -
Model 68.89 13.78 7.85 0.0087 significant
A-CR 62.08 62.08 35.35 0.0006 significant
B-CCR 1.31 1.31 0.74 0.4169 not significant
Residual
AB 0.12 0.12 0.070 0.7993 not significant
Compressive
A2 2.92 2.92 1.67 0.2379 not significant
Strength
B2 0.63 0.63 0.36 0.5670 not significant
(400 ◦ C) (MPa)
Residual 12.29 1.76 - - -
Lack of Fit 1.03 0.34 0.12 0.9422 not significant
Pure Error 11.26 2.82 - - -

The ANOVA for the residual compressive strengths models at 27 ◦ C, 200 ◦ C, and
400 ◦ C was further explained in terms of the degree of determination (R2 ) as presented in
Table 8. An R2 value of 1 (unity) implied a perfectly fitted model, while a lower R2 value
implied a model not well fitted. All of the developed models have a reasonably high degree
of correlations (R2 > 0.7), which implies that for all of the models, only less than 30% of the
experimental data could not be explained by the models. The R2 values of 0.882, 0.741, and
0.849 for residual compressive strengths models at 27 ◦ C, 200 ◦ C, and 400 ◦ C, respectively,
implied that all of the experimental data were fitted and explained by the model except
11.8%, 25.9%, and 15.1% for residual compressive strengths at 27 ◦ C, 200 ◦ C, and 400 ◦ C
models, respectively. The adjusted and predicted R2 values were further used to check the
adequacy and correlation of the models. For a good and well-fitted model, the difference
Buildings 2022, 12, 398 15 of 24

between the adjusted and predicted R2 should be less than 0.2 [39,40]. For the residual
compressive strength models at 200 ◦ C and 400 ◦ C, the difference between their predicted
and adjusted R2 values is less than 0.2. Therefore, it can be said their predicted and adjusted
R2 are reasonably in agreement with each other. However, for the residual compressive
strength model at 27 ◦ C, the difference between its predicted and adjusted R2 value is
greater than 0.2. This might be due to a problem with the model or data or might indicate a
large block effect. Therefore, model reduction through backward elimination was carried
out to remove the non-significant model terms. After model reduction, the differences
between the predicted and adjusted R2 values for the residual compressive strength model
at 27 ◦ C became less than 0.2, as shown in Table 8. The coefficient of variations (CoV)
was also used to measure the dispersion of experimental data across the predicted models.
From Table 8, the residual strength model at 200 ◦ C had the least CoV value of 2.8%, while
the residual strength model at 27 ◦ C had the highest CoV value of 4.49% (although all
of the models can be said to be lower CoV values and can therefore be used to predict
responses with lower residual error related to predicted values). The signal-to-noise levels
for each model were measured using adequate precision. Every one of the prototypes
has a good precision value of more than four. The models can be utilized to cruise the
design domain as defined by the model type selected. The developed mathematical model
after the non-significant terms was removed for residual compressive strength at 27 ◦ C is
presented as Equation (10), Where the best one-term-smaller model (insignificant term),
i.e., B (CCR) for the selected criteria was kept in order to improve the criterion score.

FC,R (27 ◦ C) = 42.91 − 0.417 × A + 1.16 × B − 0.146 × B2 (10)

where FC,R represents the residual compressive strength in MPa, A represents CR in %, and
B represents CCR in %.

Table 8. Coefficient of determination for residual compressive strength models.

Before Model Reduction After Model Reduction


Factors ◦C ◦C ◦C
27 200 400 27 ◦ C 200 ◦ C
Std. Dev. 1.76 1.05 1.33 1.60 1.05
Mean 39.21 37.49 30.10 39.21 37.49
C.V. % 4.49 2.80 4.40 4.08 2.80
PRESS 130.06 11.63 24.29 49.12 11.63
R2 0.882 0.741 0.849 0.874 0.7413
Adjusted R2 0.797 0.610 0.740 0.833 0.557
Predicted R2 0.291 0.557 0.701 0.732 0.610
Adequate
10.74 5.48 8.18 15.17 5.48
Precision

Equation (10) is the statistically fitted and modified version of Equation (9a), obtained
after Equation (9a) was subjected to model reduction through backward elimination. Based
on the ANOVA presented in Table 8, Equation (9a) cannot be used statistically to predict
the residual compressive strength of the SCC mixes at 27 ◦ C, as the difference between
the model’s predicted and adjusted R2 values must have been greater than 0.2. Therefore,
there might be a large block effect or possible problem with the model or data. Therefore,
to fix this error, model reduction by removing the insignificant terms in the model is re-
quired [39,40]. After model reduction, Equation (10) is the statistically fitted and acceptable
model that can be used to predict the residual compressive strength at 27 ◦ C for the SCC
mixes containing CR and CCR, with agreed predicted and adjusted R2 values as shown
in Table 8.
The degree of determination and correlation of the models for predicting the residual
compressive strength of the SCC mixes at temperatures of 27 ◦ C, 200 ◦ C, and 400 ◦ C were
validated graphically by plotting the normal plots against internally studentized residuals
and the predicted versus actual plots. From the normal plots against internally studentized
Buildings 2022, 12, 398 16 of 24

residuals as presented in Figure 5, all of the models followed the normal probability
Buildings 2022, 12, x distribution. They were all aligned along the straight line. Therefore, the normal12probability
of 16
distribution assumed and used for the statistical models is true. Additionally, the data
points were reasonably aligned across the linear trend line. Therefore, the experimental
results agree
resultswith
agreethe predicted
with models.
the predicted Hence,
models. the developed
Hence, model
the developed equations
model equationscan
canpredict
thepredict
residual compressive strength of the SCC mixes under normal temperature
the residual compressive strength of the SCC mixes under normal temperature (27 (27 ◦ C),
◦ C, and 400 ◦ C using CR and CCR as the variables with high degree of accuracy.
200°C), 200 °C, and 400 °C using CR and CCR as the variables with a high degree of accuracy.

(a) (b)

(c)
Figure
Figure 5. 5. Normalplot
Normal plotagainst
against internally
internally studentized
studentized residuals for for
residuals residual compressive
residual strength
compressive strength
models for (a) Control Temperature (27 °C),
models for (a) Control Temperature (27 ◦ C),(b)(b)200
200°C,◦ C,
and (c) 400 °C. ◦
and (c) 400 C.
The 3D plots of residual compressive strength models at 27 °C, 200
The 3D plots of residual compressive strength models at 27 ◦ C,°C, 200and
◦ C,400
and°C400
are◦
C are
presented in Figure 6a–c, respectively. The residual compressive strength decreased with
presented in Figure 6a–c, respectively. The residual compressive strength decreased with
an increase in elevated temperature. At all of the temperatures, the residual compressive
an strength
increasedecreases
in elevated temperature. At all of the temperatures, the residual compressive
with incrementally replacing fine aggregate with CR. At elevated tem-
strength
peratures, the decrease incrementally
decreases with replacingstrength
in residual compressive fine aggregate with CR.
with increased At elevated
substitution of tem-
peratures, the decrease in residual compressive strength with increased substitution of sand
Buildings 2022, 12, 398 17 of 24
Buildings 2022, 12, x 13 of 16

with CR can be attributed to the continuous deterioration of the rubber particles due to
sand withheat
intense CR can be attributed
resulting in poorto the continuous
bonding betweendeterioration of the rubber
the cement matrix particles
and rubber dueand
particle
tohence
intense heat resulting in poor bonding between the cement matrix and rubber
reduced strength. The addition of CCR improved the residual compressive strengths particle
and hence
of the SCCreduced strength.
mixes. This The addition
increment was more of effective
CCR improved
at higherthe residual compressive
temperatures of 200 ◦ C and
strengths
400 C. This can be as a result of the interaction of CCR with free lime to produce of
◦ of the SCC mixes. This increment was more effective at higher temperatures extra
200
CSH°C and
and 400 °C. hence
CAH, This can be as a the
reducing result of the of
amount interaction
Ca(OH)2ofandCCR anwith free lime
un-moist to pro-
portion of the
duce extrafraction
surface CSH and CAH,by
assisted hence reducingwhich
autoclaving, the amount of Ca(OH)
intensify 2 and an un-moist por-
the rheology and hence improves
tion of the surface fraction assisted
the residual compressive strength [50].by autoclaving, which intensify the rheology and hence
improves the residual compressive strength [50].

(a) (b)

(c)
Figure
Figure6. 6.
3D3D response
response surface
surfaceplot
plotfor
forresidual
residualcompressive
compressivestrength
strengthmodels
modelsfor
for(a)
(a) Control
Control Tem-
Tempera-
perature
ture (27(27 °C),
◦ C), (b)(b) 200
200 °C,and
◦ C, and(c)(c)400
400◦ C.
°C.

3.2.2.
3.2.2. Weight
Weight Reduction
Reduction dueDue to Elevated
to Elevated Temperature
Temperature
TheThe weight
weight reduction
reduction of of
thethe
SCC SCC mixes
mixes after
after subjecting
subjecting to elevated
to elevated temperatures
temperatures of of
200 ◦ C and 400 ◦ C were modelled using RSM by considering CR and CCR as the variables.
200 °C and 400 °C were modelled using RSM by considering CR and CCR as the variables.
The
The ANOVA
ANOVA summary
summary for for the generated
the generated prototype
prototype models models
is shown is shown
in Tablein9.Table 9. The
The rele-
relevance
vance of theofmodels
the models was tested
was tested utilizing
utilizing theirtheir p-values
P-values (i.e.,(i.e., p < 0.05).
p < 0.05). ThisThis is also
is also usedused
to to
Buildings 2022, 12, 398 18 of 24

prove or disprove the null hypothesis of the models. The models for the weight reductions
at 200 ◦ C and 400 ◦ C were significant with p-values below 0.05. The F-values of 164.73
and 12.09 for weight reduction models at 200 ◦ C and 400 ◦ C correspondingly show they
were all relevant against their corresponding null hypotheses. The significance of each of
the model terms can also be explained using p < 0.05. For weight reduction at the 200 ◦ C
model, only the terms CR and (CCR)2 were statistically significant in the model with p
values below 0.05. The remaining were not significant as their p values are above 0.05. For
weight reduction at 400 ◦ C models, only the model term CR is statistically significant.

Table 9. ANOVA for weight reduction due to elevated temperature models.

Sum of Mean F p-Value


Response Source
Squares Square Value Prob > F
Model 2.32 0.46 164.73 <0.0001 significant
A-CR 1.61 1.61 572.89 <0.0001 significant
B-CCR 0.0008167 80.0008167 0.29 0.6068 not significant
Weight AB 0.000025 0.000025 0.008885 0.9275 not significant
Reduction A2 0.59 0.59 209.72 <0.0001 significant
(200 ◦ C) B2 0.0004139 0.0004139 0.15 0.7127 not significant
Residual 0.020 0.002814 - - -
Lack of Fit 0.0005768 0.0001923 0.040 0.9877 not significant
Pure Error 0.019 0.004780 - - -
Model 5.51 1.10 12.09 0.0025 significant
A-CR 4.81 4.81 52.72 0.0002 significant
B-CCR 0.34 0.34 3.74 0.0944 not significant
Weight AB 0.14 0.14 1.50 0.2600 not significant
Reduction A2 0.19 0.19 2.09 0.1911 not significant
(400 ◦ C) B2 0.00002373 0.00002373 0.0002603 0.9876 not significant
Residual 0.64 0.091 - - -
Lack of Fit 0.078 0.026 0.19 0.9009 not significant
Pure Error 0.56 0.14 - - -

Still, all other model terms were not significant statistically. All of the model’s lack
fit was insignificant as their p-values were greater than 0.05. The F values of 0.04 and
0.12 for weight reductions at 200 ◦ C and 400 ◦ C models, respectively, implied 98.77%
and 90.09% probabilities for weight reductions at 200 ◦ C and 400 ◦ C models. Lack of fit
those F-values could arise due to noise. For the model to be fit, its lack of fit should be
non-significant [11,32,39]. Therefore, all of the models were said to fit well. Their lack of fit
was not significant relative to their corresponding pure errors. The developed statistical
models for the weight reductions at 200 ◦ C and 400 ◦ C are presented as Equations (11)
and (12).

WR(200 ◦ C) = 0.393 − 0.0404 × A − 0.0067 × B − 0.00005 × A × B + 0.0046 × A2 + 0.0005 × B2 (11)

WR(400 ◦ C) = 3.161 − 0.0554 × A − 0.0835 × B − 0.0037 × A × B + 0.0026 × A2 + 0.00012 × B2 (12)


where WR represents weight reduction in %, A represents crumb rubber (CR) in %, and B
represents calcium carbide residue (CCR) in %.
Table 10 presents the ANOVA summary in terms of coefficient of determination for
the weight reductions at 200 ◦ C and 400 ◦ C models. Both models have high degrees of
determination (R2 ) values. The model for weight reduction at 200 ◦ C had an R2 value of
0.992, which is very close to unity (perfect model). Only less than 1% of the experimental
data was not well fitted into the model. Similarly, the model for weight reduction at 400 ◦ C
also has a very high R2 value of 0.9, which implied only about 10% of the experimental
data was not fully and well fitted into the model.
Buildings 2022, 12, x 15 of 16

Buildings 2022, 12, 398 19 of 24


Furthermore, for both models, their adjusted and speculated R2 values were logically
in accordance with one other as their difference is below 0.2. This implied a good and
well-fitted
Table model with
10. Coefficient a high degree
of determination of accuracy
for weight [39,40].
reduction The dispersion of experimental
models.
data across the predicted models was measured using the coefficient of variations (COV).
Factors
All of the models had a low Weight
COVReduction (200 ◦8.5%.
of less than C) (%)All ofWeight Reduction
the models can be(400 ◦ C) (%)
said to be a
lower COV S value. They can therefore
0.053be used to predict the responses
0.30 with a lower
residual Mean
error related to their predicted 0.65values. The signal-to-noise levels
4.34 for each model
C.V. % using adequate precision.
was measured 8.20 Each of the model has a proper 6.96 precision value
PRESS
greater than four, meaning that the models can be utilized to cruise the1.46
0.032 design domain as
R2 0.992 0.90
defined by the model
2 type chosen.
Adjusted R 0.987 0.822
Predicted R2 0.986 0.763
Table 10. Coefficient of determination for weight reduction models.
Adequate Precision 29.50 11.05
Factors Weight Reduction (200 °C) (%) Weight Reduction (400 °C) (%)
Furthermore,
S for both models, their adjusted and speculated R2 values
0.053 0.30were logically
in accordance with one other as their difference is below 0.2. This implied a good and
Mean 0.65 4.34
well-fitted model with a high degree of accuracy [39,40]. The dispersion of experimental
C.V. % 8.20 6.96
data across the predicted models was measured using the coefficient of variations (COV).
All of thePRESS
models had a low COV of less 0.032than 8.5%. All of the models 1.46 can be said to be
R 2 0.992
a lower COV value. They can therefore be used to predict the responses 0.90 with a lower
residual Adjusted R2 to their predicted0.987
error related values. The signal-to-noise levels 0.822
for each model
Predictedusing
was measured R adequate precision.
2 0.986
Each of the model has a proper 0.763
precision value
Adequate
greater Precision
than four, meaning that the models 29.50can be utilized to cruise the 11.05 design domain as
defined by the model type chosen.
200◦°C
200 C and 400400 °C◦ Cmodels
modelswere wereverified
verifiedandandchecked
checked graphically
graphicallyby plotting the nor-
by plotting the
mal plots
normal against
plots internally
against studentized
internally residuals,
studentized as presented
residuals, in Figure
as presented 7. Both7.models
in Figure Both
models
followed followed the normal
the normal probability
probability distribution
distribution function
function as the as theplots
data data were
plots aligned
were aligned
along
along the straight
the straight trendtrend line. Therefore,
line. Therefore, the normal
the normal probability
probability distribution
distribution assumed
assumed and
and used
used forstatistical
for the the statistical
models models is true.
is true. Additionally,
Additionally, forofall
for all theofmodels,
the models, the data
the data points
points were
were reasonably
reasonably aligned
aligned acrossacross the linear
the linear trend trend line. Therefore,
line. Therefore, the experimental
the experimental results results
reason-
reasonably agree with the predicted models. Hence, the developed model
ably agree with the predicted models. Hence, the developed model equations can predict equations can
predict the weight reductions ◦
the weight reductions of theof the mixes
SCC SCC mixes
under under elevated
elevated temperatures
temperatures of 200
of 200 C and
°C and 400
400 ◦ C utilizing CR and CCR as the variables with greater accuracy.
°C utilizing CR and CCR as the variables with greater accuracy.

(a) (b)
Figure7.7. Normal
Figure Normal plot
plot against
against internally
internallystudentized
studentizedresiduals
residualsfor
forweight
weightreduction models
reduction forfor
models (a)
200 °C◦model and (b) 400 °C◦model.
(a) 200 C model and (b) 400 C model.

The3D
The 3Dplots
plotsfor
forthe
theweight
weight reduction
reduction at at
200200
◦ C°C and
and 400400
◦ C °C
areare presented
presented in Figure
in Figure 8a
8a,b,8b,respectively.
and respectively.The
Theweight
weightreductions
reductionsincrease
increase with
with increment in temperature
increment in temperaturedueduetoto
continuous deterioration of the cement matrix. Additionally, the weight reduction further
increases with the addition in partial substitution of sand using CR at all temperatures.
The weight reduction due to CR addition was more severe at 400 °C. This might be due
to the fact that the spalling due to internal pressure from heating is more severe at higher
temperatures.
Additionally, dehydration of C-S-H gels takes place under elevated temperature, and
this causes increased internal stresses and microcracks, which consequently result in in-
Buildings 2022, 12, 398 20 of 24
creased weight reduction [44,51,52]. As shown in Figure 8a, the addition of CCR does not
affect the weight reduction of the SCC when heated at 200 °C. However, at 400°C, the
addition of CCR significantly increased the weight reduction of CCR. This might be due
◦ C. This might be due
The weight reduction
to continuous due toofCR
degradation theaddition was more
excess C-S-H severe from
generated at 400the reaction of the lime
to the CCR
from fact that
andthe spalling
cement due to internal
hydration pressure
products, causingfrom heating isand
microcracks more severe of
spalling at higher
the ce-
temperatures.
ment paste, thus resulting in increased weight loss [44].

(a) (b)
Figure 8.
Figure 8. 3D3D
response surface
response plotplot
surface for weight reduction
for weight modelsmodels
reduction for (a) 200
for °C
(a)model and
200 ◦ C (b) 400
model °C
and
model. ◦
(b) 400 C model.

3.3. Multi-Objective Optimization Response


Additionally, dehydration of C-S-HAnalysis
gels takes place under elevated temperature,
and this causes increased
Multi-objective internal stresses
optimization has beenand microcracks,
carried out usingwhich consequently
response result in
surface methodol-
increased
ogy (RSM)weight reduction
to maximize the [44,51,52]. As shownperformance
sample’s durability in Figure 8a,and
theheat
addition of CCR
resilience does
contain-
not affect the weight reduction of the SCC when heated at 200 ◦ C. However, at 400 ◦ C, the
ing CR and CCR. The optimization used to obtain the best combinations of the variables
addition of CCR
that can be used significantly
to achieve theincreased
optimum theresults
weightofreduction of CCR.
performance. TheThis
CR wasmight be dueastoa
utilized
continuous degradation of the excess C-S-H generated from the reaction
partial substitution to sand. At the same time, the CCR was used as supplementary of the lime from
ce-
CCR and cement hydration products, causing microcracks and spalling
mentitious material in the SCC mix to achieve the maximum residual compressive of the cement paste,
thus resulting
strength in increased
and minimum weight
weight loss [44].after subjecting to elevated temperature. Addi-
reduction
tionally, the optimization aimed to achieve minimum water absorption and minimum
3.3. Multi-Objective Optimization Response Analysis
weight reductions after subjecting the concrete to H2SO4 and MgSO4 attacks. The optimi-
Multi-objective
zation optimizationinhas
criteria are summarized been11.
Table carried out using response
The multi-objective surface methodology
optimization results ob-
(RSM) to maximize the sample’s durability performance and heat resilience
tained from the RSM software are also presented in Table 11. The best performance containing of CR
the
and CCR. The optimization used to obtain the best combinations of the variables
SCC mixes was achieved when 2.9% fine aggregate was partially substituted with CR and that can
be used
5.5% to achieve
cement the optimum
with CCR. results
The optimal mixof proportion
performance. The CRhad
achieved wasdesirability
utilized asof a partial
77%, a
substitution to sand. At the same time, the CCR was used as supplementary cementitious
high value.
material in the SCC mix to achieve the maximum residual compressive strength and
minimum weight reduction after subjecting to elevated temperature. Additionally, the
optimization aimed to achieve minimum water absorption and minimum weight reductions
after subjecting the concrete to H2 SO4 and MgSO4 attacks. The optimization criteria are
summarized in Table 11. The multi-objective optimization results obtained from the RSM
software are also presented in Table 11. The best performance of the SCC mixes was
achieved when 2.9% fine aggregate was partially substituted with CR and 5.5% cement
with CCR. The optimal mix proportion achieved had desirability of 77%, a high value.
Buildings 2022, 12, 398 21 of 24

Table 11. Optimization criteria and results.

Lower Upper
Name Goal Solutions
Limit Limit
A:CR (%) In range 0 20 2.9
B: CCR (%) In range 0 10 5.5
Weight Reduction in H2 SO4 (28 Days) (%) minimize 3.67 10.4 6.48
Weight Reduction in MgSO4 (28 Days) (%) minimize 0.99 2.91 1.61
Water Absorption (%) minimize 1.74 2.83 1.99
Residual Compressive Strength (27 ◦ C) (Mpa) maximize 32.5 45.2 43.52
Residual Compressive Strength (200 ◦ C) (Mpa) maximize 35 39.27 38.81
Residual Compressive Strength (400 ◦ C) (Mpa) maximize 27 34.1 32.17
Weight Reduction (200 ◦ C) (%) minimize 0.36 1.43 0.29
Weight Reduction (400 ◦ C) (%) minimize 3.11 5.39 3.75
Desirability (%) 77

4. Conclusions
In this research work, response surface methodology (RSM) was utilized to design the
experiment and develop models for predicting the durability performance of SCC mixes
in terms of acid and salt attacks and the effects of elevated temperatures on the residual
compressive strength and weight of the SCC mixes. The variables considered CR a partial
sand replacement and CCR supplementary cementitious material. Hence the following
conclusions were obtained from the investigation results and interpretation:
1. The replacement of up to 10% fine aggregate with CR improved the acid resistance
of SCC measured in terms of immersion in H2 SO4 and salt resistance measured
immersion in MgSO4 . On the contrary, higher CR content decreased the acid and salt
resistance of the SCC. Similarly, partial replacement of up to 10% cement with CCR
slightly improved its acid and salt attack resistance, with higher CCR contents having
negative effects on the acid and salt attack resistance of the SCC mixes.
2. The water absorption of the SCC increased with the incorporation of CR as fine
aggregate replacement. It decreased with the addition of CCR as SCM.
3. The heat resistance of the SCC measured in weight reduction and residual compressive
strength of the SCC mixes after subjecting to elevated temperatures of 200 ◦ C and
400 ◦ C was decreased with the incorporation of CR as a fine aggregate replacement,
with the reduction more pronounced on the higher temperature.
4. The addition of CCR as cement replacement slightly improved the residual com-
pressive strength of the SCC at all temperatures. In terms of weight reduction, CCR
increased the weight reduction of the SCC at temperatures above 200 ◦ C.
5. The models generated using RSM to predict the durability performance and heat resistance
of the concrete were significant with high degrees of correlation and predictability.
6. The multi-objective optimization results showed that the best optimum or best mix
combination based on minimum weight loss in terms of H2 SO4 and MgSO4 attacks
minimum water absorption. After being subjected to elevated temperature, the
maximum residual compressive strengths and minimum weight reductions were
achieved by replacing 2.9% fine aggregate with CR and 5.5% cement with CCR.

5. Limitations, Practical Applications, and Future Research


This study was limited to normal strength SCC mixes. The CCR was obtained from
only one source. The maximum amount of CCR was limited to 10% as a partial replacement
by weight of cement, and the CR was limited to 20% as a replacement by volume of
fine aggregate. The research was also limited to utilizing CCR as a partial replacement
to cement to mitigate the negative effects of CR on the durability performance of SCC
in terms of acid attack resistance, salt attack resistance, water absorption, and effect of
elevated temperature under normal and high temperatures (27 ◦ C, 200 ◦ C, and 400 ◦ C).
The models developed using RSM can predict the weight reductions of the SCC mixes
Buildings 2022, 12, 398 22 of 24

subjected to 5% H2 SO4 and MgSO4 solutions. It can also be used to predict the weight
reductions and residual compressive strength of the SCC mixes after subjecting to normal
and elevated temperatures of acid attack resistance, salt attack resistance, and effect of
elevated temperature 27 ◦ C, 200 ◦ C, and 400 ◦ C. The models developed to apply to SCC
mixes containing 0% to 10% CCR as cement replacements and 0% to 20% CR as fine
aggregate replacements. The developed models can predict the durability performance of
SCC mixes in terms of acid and salt attack resistance and effects of elevated temperatures
using CR, CCR, and fly ash as the variables. This will reduce the need for carrying out
experimental work, hence reducing cost and time. The developed SCC mixes can construct
structures subjected to acid attacks such as industrial storage and sewage systems structures
subjected to salt attacks such as bridge piers under seas or oceans.
Future research directions include studying the effects of higher concentration and
concentration times of the acid and salt solutions on the SCC mixes. Additionally, there is a
need to study the effects of higher temperatures above 400 ◦ C and higher exposure time on
the performance of the SCC mixes containing higher CR and CCR contents.

Author Contributions: Conceptualization, O.A.U., S.E.K. and M.A.; methodology, S.E.K., M.A. and
H.A; software, S.E.K. and M.A.; validation, M.A., Y.E.I. and I.P.O.; formal analysis, S.E.K., M.A. and
H.A; investigation, O.A.U., S.E.K. and I.P.O.; resources, O.A.U., Y.E.I. and H.A.; data curation, S.E.K.
and M.A.; writing—original draft preparation, S.E.K. and M.A.; —review and editing, O.A.U., Y.E.I.
and H.A; visualization, O.A.U. and Y.E.I.; supervision, O.A.U. and Y.E.I.; project administration,
Y.E.I.; funding acquisition, Y.E.I. All authors have read and agreed to the published version of
the manuscript.
Funding: This research was supported by the Structures and Materials (S&M) Research Lab of Prince
Sultan University, Saudi Arabia. Furthermore, the authors acknowledge the support of Prince Sultan
University in paying the article processing charges (APC) of this publication.
Informed Consent Statement: Not applicable.
Acknowledgments: The authors wish to acknowledge the support of the Structures and Materials
laboratory (S&M Lab) of the College of Engineering, Prince Sultan University, Riyadh, Saudi Arabia,
and the Department of Civil Engineering Laboratory, Bayero University Kano, Nigeria, for their
vital support.
Conflicts of Interest: The authors declare no conflict of interest.

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