Construction and Building Materials 172 (2018) 635–649

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Construction and Building Materials

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

Self-compacting concrete incorporating sugarcane bagasse ash

Juliana Petermann Moretti a, Sandra Nunes b,⇑, Almir Sales a
a
Department of Civil Engineering, University of São Carlos (UFSCar), Via Washington Luís, km 235, São Carlos, SP 13565-905, Brazil
b
CONSTRUCT-LABEST, Faculty of Engineering (FEUP), University of Porto, Portugal, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal

h i g h l i g h t s

Valorization of sugarcane bagasse ash generated by the Brazilian sugarcane industry.

Sugarcane bagasse ash as a filler material in powder-type self-compacting concrete.

Mixture design method based on statistical factorial design approach.

Good mechanical and durability performance of tested self-compacting concretes.

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

Article history: The aim of the current study is to assess the feasibility of incorporating sugarcane bagasse ash (SBA) from
Received 12 December 2017 the sugar and ethanol industry as a filler material in the production of self-compacting concrete (SCC). For
Received in revised form 29 March 2018 this purpose, paste composition was designed in the first stage of this study by conducting an experimen-
Accepted 30 March 2018
tal plan at the mortar level. During the second stage, SCC mixture properties were evaluated by consid-
Available online 6 April 2018
ering the paste mixture proportions defined in the first stage. The study at the mortar level was
conducted based on a statistical factorial design approach, which offers a valid basis for developing
Keywords:
empirical models that allow determination of optimal settings of the design variables to satisfy all per-
Agricultural waste
Recycling
formance requirements. At the concrete level, the impact of three optimised paste mixtures on SCC prop-
Sugarcane bagasse ash erties was assessed. Fresh state, mechanical, and durability properties were evaluated. Mortar and
Self-compacting concrete concrete test results revealed that SBA can be used successfully in powder-type SCC as a filler material,
Statistical factorial design and it exhibits good self-compacting ability and strength levels, which are adequate for many current
civil engineering applications.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction could contribute significantly to CO2 reductions and proposed two

Concrete provides the foundation for the current built environ-
ment. This intensive use of concrete is expected to increase over
the next decades, because of increasing global population and
urbanisation rates, portending very alarming figures concerning
the environmental footprint [1]. No alternative for concrete as a
major global construction material currently exists that can be
applied at sufficient scale. The growth of market demand for con-
crete and cement is developing faster than the technical potential
to reduce CO2 emissions per ton of product; hence, absolute CO2
emissions will continue to increase. Replacing cement by other
lower carbon materials with cementitious properties was identi-
fied as one of the four levers for carbon emissions reduction by
the World Business Council for Sustainable Development [2]. In
this regard, Miller et al. examined several material alternatives that
⇑ Corresponding author.
E-mail address: snunes@fe.up.pt (S. Nunes).
clinker substitution methods: calcined clay with limestone filler
and engineered filler combined with dispersant [3]. Another chal-
lenge facing the construction sector concerns the need for a
close-the-loop approach to managing product lifecycles through
greater recycling and re-use, to reduce the environmental impacts
caused by the excessive use of natural resources. The construction
sector produces an enormous amount of waste, thus a large poten-
tial exists for a more efficient use and recycling of raw materials
[4]. This sector also offers opportunities for industrial symbiosis,
achieved by converting other industrial by-products into raw
materials for the construction sector. Concrete production, in par-
ticular, allows incorporation of several industrial and agricultural
wastes, either as partial surrogates of the aggregates or of cement.
Comprehensive reviews on the effects of different wastes on con-
crete properties can be found in the literature, comprising: indus-
trial wastes such as silica fume, fly ash, and slag [5]; waste foundry
sand, coal bottom ash, cement kiln dust, and wood ash [6]; agricul-
tural waste [7]; glass waste [8]; aggregates from construction

https://doi.org/10.1016/j.conbuildmat.2018.03.277
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
636 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649

demolition waste [9]; and various industrial by-products as partial
replacement for fine aggregate in concrete [10].
Martinera and Monzó recently presented a review paper char-
acterising the current state of development of technologies associ-
ated with recycling agricultural wastes as supplementary
cementitious materials, identifying the main research needs and
the obstacles to a widespread use of agricultural ashes [11]. Wastes
mainly from the sugar and rice industries are increasingly used as
alternative sources of fuel for industrial processes, mainly owing to
their abundant reserves of biomass; thus, they are good candidates
for massive production of vegetable ashes. These ashes, if fired
under controlled temperature and residence time, might exhibit
pozzolanic properties, enabling their use as cement substitutes in
cementitious systems (typically in proportions between 0 and
20% by mass) [11]. Besides rice husk and sugarcane ashes, the most
studied agricultural ashes, other vegetable ashes have been stud-
ied, such as corncob, wheat straw and plane leaf [12]; bamboo leaf,
corn cob, and wood waste [7]; and cassava peel [13]. Nevertheless,
it is recognised there is a need to better understand the extent to
which these vegetable ashes should be utilised in cementitious
systems based on their availability, the most appropriate process-
ing conditions, impact on durability of concrete products, and
potential to contribute to the reduction of environmental impacts
on a full life cycle basis [11].
The current work focuses on the use of sugarcane bagasse ash
(SBA) to produce self-compacting concrete (SCC). Brazil leads the
world’s sugarcane production, and in the 2015/16 harvest, 665 mil-
lion tons of sugarcane were produced [14]. Among the wastes gen-
erated in sugarcane processing, bagasse stands out owing to its
utilisation as biomass. Through the burning of bagasse, the sugar-
cane industry generates electricity for its own consumption and for
sale to electric power concessionaires. During this process, both
bottom ash (from co-generation boilers) and fly ash (from filters)
are produced. It is estimated that the bagasse corresponds to 25%
of the sugarcane production and approximately 24 kg of ashes
per tonne of bagasse burned are produced [15]. By considering
the Brazilian 2015/16 sugarcane harvest, one can estimate a gener-
ation of 4 million tons of sugarcane bagasse ashes. These ashes are
commonly deposited in landfills [16] or used as fertiliser in crops,
although they do not provide enough nutrients to be applied for
this purpose [17].
The main compound of SBA is SiO2. Thus, researchers have
explored the potential for SBA as a pozzolan in cementitious mate-
rials [18–26], aiming to reduce CO2 emissions into the atmosphere
[27]. In the pozzolanic reaction, the amorphous silica reacts with
the calcium hydroxide to form compounds with binding proper-
ties. The bagasse processing, carbon content, mineralogical compo-
sition and particle size are the main characteristics that influence
the ash’s reactivity. Table 1 presents the characteristics of several
SBA analysed in different studies. From this table, it can be con-
cluded that ashes produced under controlled temperatures and
grinding procedures can present significant pozzolanic activity
[18–23,26]. Accordingly, studies showed that SBA can be used to
produce high-strength concrete [24] or even to improve the
mechanical properties and durability of recycled aggregate con-
crete [28]. In general, if the material is fired at temperatures
around 600–700 °C, it presents amorphous silica, low loss on igni-
tion (LOI), and considerable pozzolanic activity. If the temperature
exceeds 700 °C, silica crystallization is observed [18], whose phase
composition depends on the calcination temperature and the cool-
ing conditions. Montakarntiwong et al. [26] reported on two SBAs
combusted at a controlled temperature of 800–1000 °C which
exhibited strength activity indices below 75% at 7 and 28 d; how-
ever, after grinding to increase fineness, these SBAs presented
strength activity indices above 90%, although one SBA had high
LOI (20.4%). Table 1 also presents that, in general, ashes from the

Table 1
Characteristics of several SBA analysed in different studies.

Ref. Origin Processing Particle size SiO2 (%) LOI* (%) Pozzolanic activity Recommended
(mm) use
[16] Disposal area As received D50 = 107.9 65.3 15.3 – Aggregate
[17] Boiler + filter Grinding Dmax = 600.0 62.7 16.3 – Aggregate
Boiler Grinding Dmax = 1200.0 93.5 0.3
[18] Raw bagasse burned Heating (400 °C) D50 = 12.2 – 84.5 Insufficient – 28% (NBR 5752) –
in the laboratory Heating (500 °C) D50 = 11.3 – 14.0 Insufficient – 73% (NBR 5752) –
Heating (600 °C) D50 = 11.6 61.0 5.7 Appropriate – 77% (NBR 5752) Pozzolan
Heating (700 °C) D50 = 12.3 – 3.0 Insufficient – 63% (NBR 5752) –
Heating (800 °C) D50 = 10.1 – 1.3 Insufficient – 69% (NBR 5752) –
[19] Raw bagasse burned Heating (800 °C) D50 = 12.0 69.4 1.6 High – fixed 94% of lime at 90 d Pozzolan
in the laboratory
Filter Heating (300 °C) D50 = 12.0 56.0 18.0 Low/medium – fixed 42% of lime at Pozzolan
90 d
Boiler Heating (800 °C) D50 = 18.0 66.6 4.3 Very low – fixed 11% of lime at 90 d Inert material
[20] Landfill Heating (700 °C) D50 = 20.0 56.4 10.5 – Pozzolan
[21] Boilers As received D80 = 199.0 78.34 0.42 49.5 –
Grinding 960 min tumbling mill D80 = 27.2 84.1 –
Grinding 240 min vibratory mill D80 = 5.4 103.0 Pozzolan
[22] – Grinding D50 = 10.0 64.88 8.16 113% Pozzolan
[23] Filter As received D10 = 300 72.95 21.0 72% –
Heating (700 °C) 14.0 86% Pozzolan
[24] – Grinding D50 = 16.4 65.0 10.5 – Pozzolan
[25] Boiler As received – 63.2 6.9 Free lime in pastes with ash was Pozzolan
lower than reference paste (modified
Franke method)
[26] Wet scrubber system Heating (800–1000 °C); Grinding D95 = 45.0 76.8 20.4 102% Pozzolan
Multi cyclone system 67.1 3.3 101% Pozzolan
[29] Boiler – D50 = 12.2 72.3 1.52 Low Inert material
[30] Boiler As received D50 = 40.0 73.5 – Low Filler-material
[31] Boiler Grinding Dmax = 1180.0 80.2 0.8 – Aggregate
[32] Boiler Grinding Dmax = 1200.0 80.8 0.7 Low – fixed 48 mg of CaO/g of ash Aggregate
(modified Chapelle test)
*
Loss on ignition.
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649
filters are more reactive than the ashes from co-generation boilers.
Ashes from the co-generation boilers are mainly composed of crys-
talline silica, especially quartz, owing to soil contamination [19],
and these particles negatively affect the reactivity [29]. For this
reason, researchers recommended the use of SBA from boilers as
inert material (filler/aggregate) [16,17] to be incorporated in con-
crete [30,31] and mortars [32]. More recently, a selective grinding
strategy was proposed by Cordeiro et al. [33] to reduce the content
of quartz in SBA, thus increasing the amorphous content and
improving the pozzolanic activity.
A promising field for the application of SBA from co-generation
boilers is in the production of SCC. The main characteristics of SCC
are filling ability, passing ability, and segregation resistance [34].
To ensure these characteristics, SCC usually requires the incorpora-
tion of a greater amount of filler materials than conventional con-
crete, in addition to the use of superplasticisers. SBA has the
potential to be an alternative filler material for SCC; however, only
a few studies were developed to assess the effects of incorporating
SBA into SCC. Akram et al. [35] showed the feasibility of developing
low cost SCC incorporating sugarcane bagasse ash as a viscosity
modifying agent. Five out of twenty-five concrete mixtures tested
in the fresh state were found to satisfy the requirements suggested
by EFNARC guidelines [34]. The compressive strengths of SCC with
bagasse ash at 28 d were comparable to the control concrete,
allowing a reduction of 36% in the cost of ingredients [35]. Sua-
iam & Makul [16] investigated the effect of as-received bagasse
ash (D50 = 107.9 lm) incorporation on the properties of SCC mix-
tures, when used as a partial replacement for fine aggregate. In
addition to Portland cement, a limestone waste material obtained
from the stone-crushing industry (LS) was used as fine material.
The combined use of bagasse ash and limestone powder was found
to improve workability, owing to enhanced packing density and
lower interstitial void volume, which decreases the amount of
water entrapped in the system. Therefore, SCC mixtures containing
LS and SBA required lower w/c ratios than SCC containing only SBA,
for the same workability. The optimal SCC, which contained 20% LS
and 20% replacement of the fine aggregate by SBA, showed
improved mechanical properties compared to normal SCC, while
satisfying the requirements of the EFNARC guidelines [34]. In addi-
tion to the filler effect of limestone powder, there is also a chemical
effect (the calcium carbonate can react with the aluminate
hydrates formed by cement hydration), which was found to be
more pronounced in ternary systems of cement + limestone filler
+ fly ash owing to additional aluminates provided by the fly ash
[36]. The increased volume of hydrates leads to a decrease in
Fig. 1. Particle size distribution of solid materials.
637
porosity and a subsequent increase in strength. The chemical effect
is not expected to be as pronounced in ternary systems containing
low alumina ashes, such as rice husk ash and SBA. Nevertheless,
the improvement in workability with the addition of limestone
powder allows for higher incorporation rates of low alumina ashes,
saving the clinker content, without impairing, and even improving,
compressive strength, as observed in blended systems of rice husk
ash and limestone powder [37]. Sua-iam & Makul [16] acknowl-
edged the need to further investigate the effects of SBA incorpora-
tion on the long-term mechanical and durability properties of SCC,
and to explore the synergistic effects of using binary or ternary
mixtures of fine materials (cement + SBA + other mineral addi-
tions/wastes) to improve SCC performance, reduce cement con-
sumption, and minimise material costs.
Based on the literature survey, a ternary mixture of cement +
SBA + limestone filler was selected to develop SCC mixtures. To
better understand the effects of these materials on key fresh and
hardened SCC properties and to facilitate the test protocol required
to optimise SCC, the design of experiment (DOE) approach was
selected as the frame of this study. The DOE approach represents
an improvement over the one-factor-at-a-time approach and fully
experimental methods [38]. Instead of selecting one starting mix
and then changing one factor at a time, by trial and error, to
achieve a solution satisfying all performance requirements, a set
of minimum trial experiments are defined according to established
experimental plans [39]. Experiments are then carried out, data are
collected for each response variable (relevant concrete properties,
in view of performance requirements), and the data are analysed
using standard statistical methods. These methods include fitting
numerical models to data by regression analysis, which later can
be used to determine optimal settings of the design variables using
numerical optimisation techniques. The DOE approach allows
identification of the most statistically significant effects of design
variables on responses, thereby providing a better overall system
understanding that is important for an efficient incorporation of
SBA in SCC. A similar approach was followed previously to study
the effect of recycled ground glass [40] and spent equilibrium cat-
alyst, a waste generated by the oil refinery industry [41], on SCC
mortar properties.
The aim of the current study is to assess the feasibility of incor-
porating SBA from co-generation boilers as a filler material in the
production of SCC. Hence, in the first stage of this study, paste com-
position was designed by conducting an experimental plan at the
mortar level. In the second stage, SCC mixture properties were
evaluated by considering the paste mixture proportions defined
638 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649

in the first stage. The study at the mortar level, based on a DOE 3. Research strategy
technique, consisted of the following steps: (1) selection of key
design variables and relevant response variables; (2) selection of SCC can be treated as a two-phase material, consisting of the
the type of experimental plan and the levels of design variables; paste (cement + fines + water + admixtures) and a granular phase
(3) preparation of trial batches, fabrication, and testing specimens containing all the aggregates. Aggregate particles smaller than
to collect data; (4) statistical analysis of experimental data and fit- 0.125 mm are considered as part of the fines content in SCC [34].
ting of response (numerical) models; and (5) optimisation of mix- The quality of cement paste is governed mainly by the powder
ture proportions using the fitted models. At the concrete level, an mixture, water/powder ratio, and superplasticiser dosage; how-
experimental program was developed to assess the impact of opti- ever, the amount of paste required to achieve self-compactability
mised paste mixtures on several SCC properties that comprised depends also on the characteristics of the aggregates (namely sur-
fresh state properties (sieve segregation test, J-ring test, slump- face area and voids volume in aggregates) [38]. The surface area is
flow test, and V-funnel test), mechanical properties (static modu- governed by the shape and maximum size of aggregates, whereas
lus of elasticity and compressive strength), and durability proper- the voids volume is affected mainly by the packing density of
ties (electrical resistivity, chloride ion penetration, capillary aggregates [38]. For the set of constituent materials described in
water absorption, and depth of carbonation). It is noteworthy that Section 2, SCC mixture proportions can be defined considering
no other study was found in the literature that used systematic sta- seven design variables (V w =V p ; w=c; Sp=p; SBAS=c; V s =V m ;
tistical methods for mix-designing SCC mortar/concrete incorpo- V g =V g;lim ; s1 =s) and the formulation described in [41].
rating the sugarcane bagasse ash. To reduce the number of concrete batches needed to study the
effect of all design variables that must be considered in the SCC
mix design process, initial tests are often carried out at the mortar
2. Materials level. Following the procedure described by Nunes et al. [45], in the
The materials used in this study were as follows: commercial Type I 42.5R Port-
first stage, a research program was developed at the mortar level
land cement that complies with the requirements of EN 197-1:2001, SBA, limestone
filler BetocarbÒ HP, superplasticiser SikaÒ ViscoCreteÒ 3005, fine sand, medium
Table 2
sand, limestone gravel, and tap water.
Chemical composition and physical properties of cement, SBA, and limestone filler.
In this study, the SBA samples were collected from the co-generation boilers of a
Brazilian sugarcane industry. The samples were dried at 100 ± 5 °C for 24 h and CEM I 42.5R* SBA Limestone filler*
ground for 240 min in a tumbling mill. The particle size distribution of SBA, cement,
and limestone filler measured using a laser particle size analyser can be compared Loss on ignition (LOI) (%) 2.86 1.30 –
in Fig. 2. The chemical composition and physical properties of fine materials are Insoluble residue (%) 1.30 – –
presented in Table 2. The lime consumption of SBA in a modified Chapelle test SiO2 20.50 91.3 <0.50
[42] was 132 mg of Ca(OH)2 per gram of SBA [43]. This result revealed the low poz- Al2O3 4.37 2.3 –
zolanic activity of SBA when compared to other pozzolanic materials, such as meta- Fe2O3 3.45 3.0 –
kaolin, where the minimum lime consumption must be 700 mg of Ca(OH)2 per CaO 62.36 0.4 –
gram of the metakaolin [44]. This low pozzolanic activity of SBA can be justified CaCO3 – – 98
owing to the high content of soil contamination (especially quartz) incorporated MgO 1.66 0.2 –
in ashes from co-generation boilers [19]. SO3 3.34 – –
The specific gravity values of fine sand, medium sand, and limestone gravel K2O 0.58 0.5 –
were 2.66 g/cm3, 2.66 g/cm3, and 2.63 g/cm3, respectively, and the absorption val- Na2O 0.17 – –
ues were 0.02%, 0.03%, and 0.54%, respectively. The particle size distribution of TiO2 – 0.9 –
the aggregates is also shown in Fig. 1. According to the supplier information, the Cl 0.05 – <0.001
superplasticiser presents the following properties: 26 ± 1.3% of solid content, pH S – – <0.04
= 4 ± 1, specific gravity of 1.05 g/cm3 and chloride content <0.1%. Acid-soluble sulfate – – <0.05
A standard sand was used for the study carried out at the mortar level. This is a Organic carbon – – <0.20
natural siliceous sand conforming to the standard EN 196-1 (round-shaped parti- Specific density (g/cm3) 3.08 2.69 2.70
cles having a diameter in the range of 0.08–2 mm, specific gravity of 2.63, and water *
Source: manufacturer.
absorption of 0.3%, by mass).

Ci Fi CCi EFNARC Ci Fi CCi

14 65
60
12
55
10
50
Tfunnel (s)

ρ (Ohm.m)

8 45

6 40
35
4
30
2
25
0 20
140 180 220 260 300 340 0 20 40 60 80 100
Dflow (mm) Age (d)
(a) (b)
Fig. 2. (a) Range of results of Dflow and Tfunnel; (b) evolution of resistivity over time for all mixtures in the experimental plan (water curing at 20 ± 2 °C until testing age).
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649 639

that allowed the design of SCC paste composition independently of cement weight ratio (w=c), superplasticiser to powder weight ratio
the rest of the mixture. For comparison with previous studies, stan- (Sp=p), and SBA to cement weight ratio (SBA=c). The experiments
dard sand conforming to EN 196-1 was employed at this stage. were designed according to a central composite design (CCD) con-
Hence, a proper experimental plan based on a DOE approach was sisting of a 24 factorial design with 16 runs, plus eight axial runs,
selected to explore the relationships between the responses and six central runs. The effects of these four design variables were
(slump flow diameter, V-funnel flow time, compressive strength, evaluated at five levels: /, 1, 0, +1, +/. According to Mont-
electric resistivity, and porosity accessible to water) and the design gomery [39], the / value depends on the number of points in the
variables (V w =V p ; w=c; Sp=p; SBA=c). After establishing explicit factorial design and must be equal to nf
1=4
to ensure the rotatability
relationships between the response variables and design variables, of the model. In this study, nf ¼ 16 thus leads to /¼ 2. The combi-
the optimal settings of the design variables were established (using nations of the levels of the four design variables for all 30 trial mix-
optimisation techniques) and validated, as described in Section 4. tures of the CCD plan are listed in Table 3. Table 4 presents the
In the second stage of this study, three SCC mixtures were correspondence between coded and actual values of the five levels
defined by fixing the paste mix proportions obtained from opti- for each design variable. For each trial mixture, mortar proportion-
mised mortars and replacing standard sand by real aggregates ing was obtained using the formulation presented in [41], and set-
(two fine aggregates and a coarse aggregate, as presented in Sec- ting V g =V g;lim and s1/s equal to 0 and 1, respectively. The sand to
tion 2). The values of V s =V m ; V g =V g;lim ; s1 =s, which allow definition
mortar volume ratio (V s =V m ) was set equal to 0.475 for all
of the aggregate skeleton and aggregates content, were set based mixtures.
on a previous study [46]. Next, trial batches were prepared, and
tests were carried out to characterise both fresh and hardened
4.2. Preparation of trial batches, fabrication, and testing of specimens
state properties of these three mixtures. The study carried out at
the concrete level is described in Section 5.
Mortar mixes were prepared in the laboratory in 1.6 L batches
Based on these studies, conclusions were drawn concerning the
and mixed in a two-speed mixer in compliance with EN 196-1
feasibility of incorporating SBA in SCC, which are presented in
[47]. The sequence of mixing consisted of the following: add refer-
Section 6.
ence sand + SBA + limestone filler + cement + 70% of the mixing
water and mix for 60 s; stop to scrape adhering material and mix
4. Study at the mortar level
for 60 s more; stop to add superplasticiser + 30% of the water and
mix for another 60 s; stop to scrape adhering material and mix
4.1. Experimental plan, design variables, and levels of design variables
for 30 s; stop for 5 min and, lastly, mix for 30 s more. Mixing was
performed at low speed, except during the last 30 s which was per-
At the mortar level, the effects of four key design variables were
formed at high speed.
investigated: water to powder volume ratio (V w =V p ), water to
The V-funnel and mortar flow tests proposed by Okamura &
Table 3 Ouchi [48] were carried out to characterise mixtures in the fresh
Experimental plan (variables in terms of coded values). state. After mixing, the V-shaped funnel was filled, and the time
taken for it to flow through the apparatus was measured. This test
Ref. Point type Vw/Vp w/c Sp/p SBA/c
was repeated twice, and the average flow time was taken as the
Ca Central 0 0 0 0
final test result (Tfunnel). Next, the mortar flow test was carried
F1 Factorial 1 1 1 1
F2 Factorial 1 1 1 1 out to assess mortar deformability by calculating the flow diameter
F3 Factorial 1 1 1 1 as the mean of two diameters in the final spread area. This test was
F4 Factorial 1 1 1 1 also repeated twice, and the mean of four diameters was consid-
F5 Factorial 1 1 1 1 ered as the final test result (Dflow). After the fresh mortar tests,
F6 Factorial 1 1 1 1
F7 Factorial 1 1 1 1
five prisms (40  40  160 mm3) and three cylinders (50 mm
F8 Factorial 1 1 1 1 diameter  30 mm height) were moulded: three prisms to evalu-
F9 Factorial 1 1 1 1 ate resistivity over time and compressive strength at 28 d; two
F10 Factorial 1 1 1 1 prisms to evaluate resistivity over time and compressive strength
F11 Factorial 1 1 1 1
at 91 d; and three cylinders to assess the porosity accessible to
F12 Factorial 1 1 1 1
F13 Factorial 1 1 1 1 water. The specimens were kept in the moulds for 24 h and subse-
F14 Factorial 1 1 1 1 quently kept under water in a special chamber (temp. = 20 ± 2 °C)
F15 Factorial 1 1 1 1 until testing age.
F16 Factorial 1 1 1 1 The electrical resistivity test is a very simple, rapid, and non-
CC1 Axial 2 0 0 0
CC2 Axial 2 0 0 0
destructive technique that provides important information about
CC3 Axial 0 2 0 0 the microstructural development of cementitious materials. This
CC4 Axial 0 2 0 0 electrical property characterises the difficulty of ion movement
CC5 Axial 0 0 2 0 in concrete/mortar [49]. The resistivity results are related to con-
CC6 Axial 0 0 2 0
crete properties such as diffusivity, permeability, and pore connec-
CC7 Axial 0 0 0 2
CC8 Axial 0 0 0 2 tivity, which strongly influence concrete durability [50]. In this
study, the mortar’s resistivity was measured through the two elec-
a
Trial mixture corresponding to central point was replicated six times.
trodes technique as described in [40]. During casting, two stainless

Table 4
Correspondence between coded and actual values for each design variable.

Design variables Low axial (2) Low factorial (1) Central 0 High factorial (+1) High axial (+2)
Vw/Vp 0.750 0.825 0.900 0.975 1.050
w/c 0.350 0.400 0.450 0.500 0.550
Sp/p 0.45% 0.55% 0.65% 0.75% 0.85%
SBA/c 0.00% 7.50% 15.00% 22.50% 30.00%
640 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649
steel networks were embedded in the mortar sample at the ends of
the prismatic specimens (40  40  160 mm3) to function as elec-
trodes. The resistivity values were obtained as follows (Eq. (1):
V:A
q¼
L:I
where V is the potential difference (volt); I is the current intensity
(amp); q is the electrical resistivity (Xm); L is the distance between
electrodes (m); and A is the area of the electrode in contact with the
mortar sample (m2). The resistivity test was carried out in all five
prismatic specimens at 7, 14, 21, and 28 d. At 28 d, three prisms
were tested to assess compressive strength; thus, only two prisms
remained to perform resistivity tests at the ages of 56 and 91 d,
and compressive strength test at 91 d. Because all the specimens
were at the same moisture (saturated) and temperature conditions,
the resistivity measure can be used to compare the amount and
interconnectivity of the matrix pores, serving as a durability indica-
tor. The mortar compressive strength test was carried out according
to EN 196-1 [47].
The porosity accessible to water was also investigated. This is
also an important indicator of the durability properties of the
material. Tests were carried out after 28 d of wet curing on
cylindrical specimens (50 mm diameter  30 mm height). The
conditioning of the mortar specimens consisted of 4 h of vacuum
(10–50 mbar pressure) and 1 h of additional vacuum with
specimens under deaerated water, followed by 18 h of soaking in
water. After conditioning, the mass of the saturated sample
weighed in air (M air ) and its hydrostatic mass (M hydr ) were deter-
mined. Next, specimens were allowed to dry in a ventilated heater
at 105 ± 1 °C. The samples were maintained at that temperature
until the mass stabilised (Mdry ,), which occurred when two consec-
utive weighings, separated by 24 h, did not differ by more than
0.05%. The following equation (Eq. (2) was used to compute the
porosity (por):
M air  Mdry
por ¼  qwater
M air  M hydr
4.3. Collected experimental data and discussion
Fig. 2(a) shows the T-funnel flow time (Tfunnel) versus slump
flow diameter (Dflow) obtained for the tested mortar mixtures.
As expected, these results show an increasing trend in slump-
Ci Fi CCi
90
80
fcm (MPa)
70
60
50
40
0 20 40 60
Age (d)
(a)
Fig. 3. (a) Evolution of compressive strength from 28 to 91 d; (b) fcm, 28 d and porosity accessible to water at 28 d, for all mixtures in the experimental plan.
flow diameter with a corresponding reduction in flow time. The
implemented experimental plan included mortars with Dflow
ranging from 153 to 326 mm and Tfunnel ranging from 2.6 to
12.5 s. These ranges of Dflow and Tfunnel appear to be adequate,
ð1Þ because these intervals include target intervals for Dflow and Tfun-
nel of 240–260 mm and 3–7 s, respectively, according to EFNARC
recommendations [34].
The evolution of the mortar’s electrical resistivity up to 91 d is
presented in Fig. 2(b). It can be observed that the largest evolu-
tion of resistivity increase occurred up to 28 d. From 28 to 91 d,
an increase of only 15–28% in resistivity was observed, consider-
ing all mixtures in the experimental plan. Similar mortar mix-
tures incorporating pozzolanic materials often exhibit much
higher increments in resistivity from 28 to 90 d, as reported by
Nunes & Costa [41]. The range of results for compressive strength
increases varied from 7 to 17%, from 28 to 91 d, as represented in
Fig. 3(a).
The porosity accessible to water results are plotted against
compressive strength at 28 d in Fig. 3(b). It is known that the
porosity is directly related to the durability of concrete, because
aggressive agents access the interior of the material through the
porous structure. From Fig. 3(b), it is possible to observe that sim-
ilar compressive strength results can be obtained for a range of
porosity values. This indicates that although these mixtures exhibit
similar compressive strength, their durability might be different
owing to higher or lower vulnerability to the attack of aggressive
agents.
Given the fact that compressive strength and resistivity did not
increase significantly from 28 to 91 d, we decided to model the
hardened mortar properties at 28 d. The average test results of
Dflow, Tfunnel, compressive strength at 28 d (fcm, 28 d), resistivity
at 28 d (q, 28 d), and porosity accessible to water (por, 28 d) for
each mixture of the experimental plan are listed in Table 5.
4.4. Statistical analysis of data and fitting of response models
ð2Þ
Descriptive statistical parameters of all the experimental results
used in the modelling, as well as those for only the central points,
are presented in Table 6. Six replicate runs of central points
allowed evaluation of the experimental error associated with each
response variable. From Table 6 and Figs. 2 and 3, it can be
observed that variation found in results of the total points is signif-
icantly higher than the variation found in the results of only the
Ci Fi CCi
20
19
por, 28d (%)
18
17
16
15
80 100 50 55 60 65 70 75
fcm, 28d (MPa)
(b)
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649 641

Table 5
Experimental test results used in the modelling.

Run number Point type Dflow (mm) Tfunnel (s) q, 28 d (Ohmm) fcm, 28 d (MPa) por, 28 d (%)
1 C1 239.50 4.99 38.17 62.03 18.12
2 C2 256.50 4.50 36.80 60.82 18.50
3 C3 264.25 3.93 38.23 62.35 18.46
4 C4 254.75 4.83 38.74 62.62 18.08
5 C5 252.50 4.48 39.62 61.77 18.31
6 C6 247.75 5.04 38.41 61.86 18.11
7 F1 159.75 12.46 46.31 69.19 16.98
8 F2 201.50 4.35 38.98 65.11 19.04
9 F3 249.75 5.42 35.07 56.72 17.75
10 F4 252.50 3.28 32.05 56.88 19.31
11 F5 240.75 7.29 45.51 69.84 16.73
12 F6 253.50 4.44 39.98 66.98 18.26
13 F7 316.25 4.55 36.95 59.91 16.43
14 F8 318.75 2.97 33.42 58.61 17.70
15 F9 165.25 10.03 44.41 68.65 17.64
16 F10 203.00 4.78 42.14 64.01 18.05
17 F11 229.75 5.60 36.77 56.93 17.88
18 F12 248.25 3.59 33.39 54.29 19.15
19 F13 213.50 8.19 45.16 67.56 16.90
20 F14 265.75 3.81 40.72 67.41 17.87
21 F15 317.50 4.50 36.75 59.65 16.93
22 F16 326.50 2.58 34.24 57.33 16.56
23 CC1 229.25 8.80 42.27 61.60 16.90
24 CC2 269.50 2.77 35.42 61.37 18.93
25 CC3 153.25 10.72 46.11 76.81 17.25
26 CC4 326.00 3.10 32.34 54.02 17.26
27 CC5 168.00 7.53 38.30 59.44 18.24
28 CC6 318.75 4.41 39.90 64.22 17.45
29 CC7 248.25 4.66 37.69 62.89 18.63
30 CC8 248.25 4.98 38.20 60.67 18.15

Table 6
Statistical results for the total (30) and central (6) points.

Dflow (mm) Tfunnel (s) q, 28 d (Ohmm) fcm, 28 d (MPa) por, 28 d (%)

N = 30 total points
Minimum 153.25 2.58 32.05 54.02 16.43
Maximum 326.50 12.46 46.31 76.81 19.31
Mean 247.96 5.42 38.74 62.38 17.85
Standard deviation 48.84 2.45 4.01 5.03 0.79
Coefficient of variation (%) 19.70 45.15 10.36 8.06 4.41
nc = 6 central points
Minimum 239.50 3.93 36.80 60.82 18.08
Maximum 264.25 5.04 39.62 62.62 18.50
Mean 252.54 4.63 38.33 61.91 18.26
Standard deviation 8.37 0.42 0.92 0.62 0.19
Coefficient of variation (%) 3.32 9.02 2.40 1.00 1.02

central points, which is a necessary (but not sufficient) condition
for finding a good fitting model.
A CCD allows for the estimation of a full quadratic model as fol-
lows (Eq. (3):
X
k X
k XX
y ¼ b0 þ bi xi þ bii x2i þ bij xi xj þ e
i¼1 i¼1 i<j
where y represents the response variable; xi corresponds to the
design variables considered; b is used for model parameters (b0 is
the independent term, bi represents the linear effect of xi , bii repre-
sents the quadratic effect of xi , and bij represents the linear-by-
linear interaction between xi and xj ); and e is the residual error term.
The model parameters (b0, bi, bij) can be estimated by means of a mul-
tilinear regression analysis, which was performed using commercial
software Design-Expert [51]. A comprehensive explanation of all
steps involved in model identification is provided in [39].
Table 7 presents the estimated model coefficients in terms of
actual values of design variables, including the residual error term
(e), along with the coefficients of determination. ANOVA pinpointed
that these models are significant when describing the effect of
V w =V p , w=c, Sp=p, and SBA=c on the modelled responses. Because
R2 and R2adjusted values are significantly high (>0.80 for por, 28 d and
>0.95 for all the remaining responses), the large proportion of the vari-
ability of response variables is explained by the obtained regression
ð3Þ
models. Residual analysis did not reveal a reason to suspect violation
of the independence, centrality, or constant variance assumptions. A
variable transformation of the form (1/y0.5) was used to stabilise both
the Tfunnel and q, 28 d response variance and improve the resulting
model, as indicated in Table 7. Because the residual standard devia-
tion of the derived models (see Table 7) does not greatly exceed the
standard deviation calculated from the central points (experimental
error) presented in Table 6, a good fit can be expected.
4.5. Significant effects on the response variables
From the estimates of the model coefficients obtained for the
coded variables, the relative influence of each design variable on
642 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649

Table 7
Fitted numerical models corresponding to actual values of design variables.

Response variable Dflow (mm) [Tfunnel (s)]0.5 [q, 28 d (Xm)]0.5 fcm, 28 d (MPa) por, 28 d (%)
Model terms Estimate Estimate Estimate Estimate Estimate
Independent 1202.04 1.406 0.0428 182.289 28.622
Vw/Vp 981.32 (12%) 0.902 (43%) 0.0521 (33%) 10.161 (9%) 13.989 (29%)
w/c 2427.71 (42%) 1.132 (36%) 0.159 (67%) 417.817 (62%) 127.392 (1%)
Sp/p 351.77 (39%) 1.436 (16%) NS 10.446 (13%) 21.258 (23%)
SBA/c NS NS NS 6.583 (6%) 40.189 (5%)
Vw/Vp  w/c 1862.50 (8%) NS NS NS NS
Vw/Vp  SBA/c NS NS NS NS 46.000 (14%)
w/c x Sp/p NS NS NS NS 56.500 (15%)
(w/c)2 NS NS NS 349.417 (10%) 100.500 (14%)
(Sp/p)2 NS 0.912 (6%) NS NS NS
e, mean 0 0 0 0 0
e, standard deviation 8.409 0.0187* 0.00183* 0.927 0.301
R2/R2adjusted 0.970/0.965 0.952/0.944 0.951/0.947 0.966/0.958 0.853/0.807

Notes: (NS) non-significant terms; values inside parentheses correspond to the relative influence of the variable on the response variation; the most significant variable is
typed bold.
*
Corresponding value for Tfunnel and q, 28 d is 0.671 and 0.879, respectively.

the responses was computed and is presented (in parentheses) in
Table 7. The results clearly show that w=c is the variable with
the higher effect on almost all the response variables, exceeded
only by the effect of V w =V p on Tfunnel and por, 28 d responses.
The superplasticiser dosage was also found to be significant for
almost all mortar properties except q, 28 d. Significant quadratic
terms on w=c and Sp=p were found for fcm, 28 d and por, 28 d,
and Tfunnel responses.
Within the range of SBA=c values selected for this study, this
variable had no significant effect on mortar fresh state properties
or mortar resistivity. The SBA=c was found to be significant only
for the compressive strength, and yet its effect is relatively small.
At 28 d, an increase of SBA=c led to a reduction of compressive
strength. The predominant effect of w=c over SBA=c on fcm, 28 d
response can be observed in Fig. 4. This effect can be explained
by the low pozzolanic activity of this material owing to the high
content of soil contamination. An interaction effect between
V w =V p and SBA=c also had a significant influence on the porosity
accessible to water, which can be visualised in Fig. 5. Porosity
increases with SBA=c for higher values of V w =V p ; however, the
opposite occurs for lower values of V w =V p .
4.6. Optimisation of mixture proportions
Based on the fitted numerical models presented in Table 7, the
numerical optimisation module implemented in Design-Expert
[51] was used first to determine the range of mortar mixture
parameters that would lead to adequate SCC mixtures (with Dflow
between 250 and 260 mm and Tfunnel between 6 and 8 s). The
optimal settings of design variables for different levels of Sp=p
are represented by the region in grey in Fig. 6. As the superplasti-
ciser dosage increases, the optimum region for SCC moves down
and to the right in the graph; indicating that higher Sp=p allows
for lower w=c and higher V w =V p while keeping the mortar’s work-
ability. It should be noted that since SBA=c had no significant effect
on both Dflow and Tfunnel responses, its level has no influence in
the optimum region found for SCC.
Fig. 6 clearly shows that a number of mortar compositions can
be found that satisfy the requirements of self-compactability. To
select a single mixture that leads to the best overall performance,
additional practical constraints should be added that take into con-
sideration other performance requirements, such as typical
requirements in terms of strength and durability (or other relevant
engineering properties for a particular application), cost, and eco-
efficiency. In accordance with the aim of this study to improve

69
19.00

65.75
18.57
fcm,28d (MPa)

62.5
por,28d (%)

18.15

59.25
17.73

56
17.30

0.07
0.23
0.11
0.40 0.19 0.97
0.15
0.43 0.94
SBA/c 0.45
0.15
0.19 0.90
0.47 SBA/c 0.11
0.23 0.86
0.50
w/c 0.07 0.82 Vw/Vp

Fig. 4. SBA/c and w/c influence on compressive strength of mortars at 28 d (Vw/Vp Fig. 5. Interaction effect between V w =V p and SBA=c on por, 28 d response (Sp/p and
and Sp/p fixed at 0.900 and 0.65%, respectively). w/c fixed at 0.65% and 0.45, respectively).
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649 643

0.55 0.55

Dflow: 260

0.50 Dflow: 250

0.50

Dflow: 260
w/c

w/c
0.45
Tfunnel: 6 Dflow: 250
0.45
Tfunnel: 6
Tfunnel: 8

Tfunnel: 8

0.40 0.40

0.35 0.35
0.750 0.825 0.900 0.975 1.050 0.750 0.825 0.900 0.975 1.050

Vw/Vp Vw/Vp
(a) Sp/p = 0.55% (b) Sp/p = 0.65%

0.55 0.55

0.50 0.50
w/c

w/c

0.45 0.45

Tfunnel: 6 Tfunnel: 6
Dflow: 260
Tfunnel: 8 Dflow: 250 Tfunnel: 8
0.40 0.40
Dflow: 260
Dflow: 250

0.35 0.35
0.750 0.825 0.900 0.975 1.050 0.750 0.825 0.900 0.975 1.050

Vw/Vp Vw/Vp
(c) Sp/p = 0.75% (d) Sp/p = 0.85%
Fig. 6. Optimum region for SCC for different levels of Sp/p.

SCC sustainability by saving energy, reducing the use of expensive
components like cement and mineral additions (finely ground, like
limestone filler) for concrete production, and improving concrete
durability, SCC-mortars selection was performed using the criteria
listed in Table 8. The w/c was fixed at three different levels target-
ing different compressive strength levels. In addition to setting the
limits for Dflow and Tfunnel to achieve self-compactability, the
goals of maximising resistivity and minimising porosity were con-
sidered for each w/c level to improve mixture durability. A goal of
maximising SBA=c was also included to increase SBA content in the
mixtures. Because SBA is a polluting waste material, a higher con-
tent of SBA in the mixture contributes both to reducing its cost and
to increasing its eco-efficiency. An additional constraint should be
implemented because the error function that is associated with
each response model increases relative to the increase in distance
to the centre of the experimental region [39]. To avoid finding
solutions too distant from the centre of the experimental region,
SBA=c was limited in range [7.5%, 22.5%]. The resulting optimised
mixtures and predicted responses are presented in Table 9. It is
interesting to notice that all mixtures have the maximum SBA=c
permitted of 22.5% owing to the relatively small influence of this
variable on the analysed responses.
To assess the validity of the developed regression models, trial
batches using the optimised mixtures were prepared and tested.
The experimental results obtained are also included in Table 9.
The ratio between predicted-to-measured values for Dflow; Tfun-
nel; q, 28 d; fcm, 28 d; and por, 28 d were very close to 1.0, ranging
between 0.87 and 1.07. One can observe that all points fall within
or are very close to the limits of the prediction intervals, which
indicate the obtained models had good accuracy.
It is worth mentioning that the obtained models are specific to
the set of materials and range of proportions used. Nevertheless,
644 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649

Table 8
Final optimisation constraints.

Mixture A B C
Design Variables:
Vw/Vp In range [0.750, 1.050] In range [0.750, 1.050] In range [0.750, 1.050]
w/c Equal to 0.40 Equal to 0.45 Equal to 0.50
Sp/p In range [0.45%, 0.85%] In range [0.45%, 0.85%] In range [0.45%, 0.85%]
SBA/c Maximise in [7.5%, 22.5%] Maximise in [7.5%, 22.5%] Maximise in [7.5%, 22.5%]
Response Variables:
Dflow (mm) In range [250, 260] In range [250, 260] In range [250, 260]
Tfunnel (s) In range [6,8] In range [6,8] In range [6,8]
q, 28 d (Ohm.m) Maximise Maximise Maximise
fcm, 28 d (MPa) None None None
por, 28 d (%) Minimise Minimise Minimise

Note: Importance was set equal for all constraints.

Table 9
Optimised mixtures, predicted and measured test results.

Vw/Vp w/c Sp/p SBA/c Dflow (mm) Tfunnel (s) q, 28 d (Ohmm) fcm, 28 d (MPa) por, 28 d (%)
0.825 0.40 0.84% 22.5% Predicted 260.00 8.00 44.80 70.00 17.17
95% PI low* 238.46 6.08 42.43 67.59 16.26
95% PI high* 281.54 10.99 47.37 72.41 18.08
Measured 256.75 8.07 51.51 65.59 15.98
Pred./Meas. 1.01 0.99 0.87 1.07 1.07
0.761 0.45 0.74% 22.5% Predicted 260.00 8.00 42.13 63.55 17.08
95% PI low* 239.48 6.27 39.92 61.17 16.20
95% PI high* 280.52 10.56 44.53 65.92 17.95
Measured 261.00 8.31 47.25 62.78 16.17
Pred./Meas. 1.00 0.96 0.89 1.01 1.06
0.732 0.50 0.60% 22.5% Predicted 260.00 8.00 38.84 58.10 17.45
95% PI low* 236.33 6.22 36.79 55.67 16.52
95% PI high* 283.67 10.68 41.06 60.54 18.38
Measured 253.50 7.69 43.17 57.20 16.35
Pred./Meas. 1.03 1.04 0.90 1.02 1.07

Note: (*) Lower and higher limits of prediction interval with 95% confidence level.

the relative trends found for this specific mixture of cement + SBA for this specific set of aggregates were established in a previous
+ limestone filler should remain consistent when a different set of study for a mortar with similar workability [46]. Thus, using the
similar materials is used. Furthermore, it is well known that small values of the design variables listed in Table 10, concrete mix-
batch-to-batch changes, like variations in cement or mineral addi- proportions could be obtained using the formulation presented in
tions caused by changes in the production process, can have a sig- [41]. Except for a 10% increase in superplasticiser dosage (to
nificant effect on the workability and evolution of hydration account for a certain amount of superplasticiser being absorbed
reactions, especially with superplasticised mixes [52]. When using by the aggregates), no further change was introduced to the opti-
agricultural waste materials, such as SBA, the situation could be mal design variable values presented in Table 9.
even worse owing to potentially higher variation in material prop-
erties and/or presence of chemical elements which interfere with
the behaviour of superplasticisers. Changes in the type of chemical
Table 10
admixtures, mixing regime, temperature, or time of addition of Mixture design variables and mix-proportions of studied mixtures.
superplasticiser can also significantly affect rheology and early
SCC-A SCC-B SCC-C
hydration kinetics of SCC [53]. The optimised mixtures presented
in Table 9 (incorporating reference sand) are useful to assess the Design variables
workability and strength variations in different deliveries of the w/c 0.400 0.450 0.500
Vw/Vp 0.825 0.761 0.732
constituent materials; and can be used to implement an efficient Sp/p 0.84% 0.74% 0.60%
quality control plan at the production centre [52]. SBA/c 0.225
Vs/Vm 0.423
s1/s 0.200
5. Study at the concrete level Vg/Vg,lim 0.525
Va 0.020

5.1. SCC mix proportions Constituent materials (kg/m3)

Cement 431.99 367.25 323.08
Limestone filler 89.58 181.27 240.02
At the concrete level, three SCC mixtures were defined by fixing
SBA 97.20 82.63 72.69
the paste mix proportions obtained from the optimised mortars Water 173.66 166.53 163.43
(see Table 9) and replacing standard sand by real aggregates Superplasticiser 5.208 4.675 3.824
(two fine aggregates and a coarse aggregate, presented in Sec- Fine sand 148.89
Medium sand 595.56
tion 2). The values of V s =V m ; V g =V g;lim ; s1 =s, (see Table 10), which
Limestone gravel 835.75
allow definition of the aggregate skeleton and aggregates content
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649 645

5.2. Mixing sequence and test methods
Mixes were prepared in the laboratory in 45 L batches and
mixed in an open pan mixer. The mixing sequence consisted of
mixing both sands and limestone gravel with 25% of the mixing
water for 2.5 min, waiting for 2.5 min for absorption and adding
of the powder materials, followed by adding the remaining water
with the superplasticiser and mixing the concrete for an additional
5 min, stopping to scrape adhering material, and, finally, further
mixing for 3 min. J-ring, slump-flow, V-funnel, and sieve segrega-
tion tests were then carried out to characterise the fresh state fol-
lowing this mixing sequence.
After testing fresh concrete, five cylinders (150 mm diameter 
300 mm height) and 4 cylinders (100 mm diameter  100 mm
height) were moulded to assess concrete hardened properties.
These specimens were demoulded one day after casting and there-
after kept under water in a special chamber (Temp. = 20 ± 2 °C)
until testing at the specified ages (see Table 11).
Concrete electrical resistivity was assessed by the two-
electrode (direct test) and four-electrode (Wenner probe) methods,
both on cylindrical specimens (/ = 150 mm; h = 300 mm). For the
direct test, low frequency electrical current passes between the
two electrodes (two stainless steel plates) while the voltage drop
is measured. Specimens were removed from the curing chamber
only a few seconds before the start of the test. Each specimen
was wiped with a damp cloth to remove excess surface water. To
ensure good electrical contact between the specimen and elec-
trodes, a wet sponge was positioned, and a force was applied to
maintain a constant and uniform stress distribution over the entire
face of the specimen (see Fig. 7(a)). Resistivity was obtained from
the electrical resistance (calculated from the potential response
using Ohm’s law) and a geometric factor, applying Eq. (4). The
four-electrode method is currently the most widely used technique
for field concrete resistivity measurements. The Wenner array
probe consists of a set of four points, each spaced a constant dis-
tance (a) apart. The current is applied between the two outer
points, while the inner two points measure the potential (Fig. 7
(b)). This has the advantage of eliminating the influence of polari-
sation as the actual potential is measured across an inner region. A
commercially available four-point resistivity meter (Canin, Proceq)
was used in this study, with a fixed electrode spacing of 50 mm.
The resistivity can be calculated using the following equation
(Eq. (3)
P
q ¼ 2pa ð4Þ
I
where q is the resistivity in Xm, a is the distance between points in
m, P is the measured potential in volts, and I is the applied current
in amperes. Resistivity measurements were carried out at 7, 14, 21,
and 28 d. Because all the specimens were at the same moisture (sat-
urated) and temperature conditions, resistivity testing provides
information about pore connectivity and the resistance of concrete
to the penetration of liquid or gas substances. After the resistivity
test at 28 d, the elasticity modulus and compressive strength were
assessed.
The corrosion of rebars embedded in concrete, owing to the
penetration of chloride ions, occurs in many different structures.
Therefore, chloride resistance is one of the most important proper-
ties of concrete to be considered at the mix-design stage. Resis-
tance to chloride penetration was evaluated by the CTH rapid

Table 11
Testing plan for concrete mixtures.

Test Reference standard/Recommendation Testing age Number/Type of specimens

J-ring (16 rebars) EN 12350-12: 2010 [54] After mixing Fresh concrete sample
Slump-flow EN 12350-8: 2010 [55]
V-funnel EN 12350-9: 2010 [56]
Sieve segregation EN 12350-11: 2010 [57]
Resistivity: Polder [58] 7, 14, 21 and 28 d 4 cylinders (/ = 150 mm; h = 300 mm)
- two-electrode Wenner method
- four-electrode
Compressive strength EN 12390-3: 2009 [59] 28 d
Elasticity modulus DIN 1048-5 [60] 28 d
Resistance to chloride penetration LNEC E 463 [61] 28 d 3 discs (/ = 100 mm; h = 50 mm) cut from the inner
part of 3 cylinders (/ = 100 mm; h = 100 mm)
Water absorption by capillarity RILEM TC 166-PCD [62] 28 d 4 discs (/ = 150 mm; h = 50 mm), cut from the inner
part of one cylinder (/ = 150 mm; h = 300 mm)
Carbonation LNEC E 391 [63] 76 d 1 cylinder (/ = 100 mm; h = 100 mm)

Fig. 7. Application of resistivity test methods: (a) two-electrode; (b) four-electrode (Wenner probe).
646 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649

Table 12
Fresh and hardened state test results.

SCC-A SCC-B SCC-C

Fresh state
Flow diameter (mm) 660 [SF2] 730 [SF2] 600 [SF1]
T500 (s) 1.9 [VS1] 1.9 [VS1] 2.8 [VS2]
V–funnel (s) 8.9 [VF1] 8.3 [VF1] 14.0 [VF2]
Flow diameter with J-ring (mm) 610 710 580
T500 with J-ring (s) 3.2 2.3 3.8
J-ring step (16 rebars) (mm) 15 13 27
Segregation índex (%) 5 [SR2] 9 [SR2] 5 [SR2]
Hardened state
Resistivity, 28 d* (Ohmm) 131.7 (2.2%) 116.3 (9.7%) 113.8 (5.8%)
Static modulus of elasticity, 28 d (GPa) 43.7 (1.7%) 45.4 (1.1%) 44.0 (1.6%)
Compressive strength, 28 d (MPa) NA 51.9 (1.9%) 47.9 (2.0%)
Chloride diffusion coefficient (1012 m2 s1) 10.82 (3.2%) 11.57 (9.7%) 13.90 (–)
Sorptivity (kg/m2  h0.5) 0.356 (5.1%) 0.378 (6.3%) 0.378 (4.1%)
Depth of carbonation (mm) 3.3 (15%) 6.5 (21%) 8.5 (12%)

Notes: (*) Corresponding to 4-electrode method; (NA) result is not available; consistency classes are indicated inside square
brackets; values inside parentheses refer to the coefficient of variation of results.

Fig. 8. Final spread area of mixtures: (a) SCC-A, (b) SCC-B, and (c) SCC-C.
 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649 647

method described in NT BUILD 492, according to Portuguese LNEC
E 463 specification [52]. This non-steady state migration method
allows calculation of the chloride diffusion coefficient.
Absorption by capillarity testing was also carried out following
the procedure described in RILEM TC 116-PCD [62]. After the sam-
ples were dried in a ventilated heater at 40 ± 5 °C until a constant
mass, test specimens were placed in a shallow water bath. The
water level was adjusted automatically so that the concrete face
was dipped to a constant depth of approximately 3 mm. From
the start of testing, water intake by capillary suction was measured
at time intervals up to four hours. Absorption of water into con-
crete under capillary action is dependent on the square-root of
time and may be modelled as follows (Eq. (5):
Resistance to carbonation was evaluated following the proce-
dure described in the Portuguese specification LNEC E 391 [63].
For each SCC mixture, a cylindrical specimen (/ = 100 mm; h =
100 mm) was subjected to wet curing for 28 d, and then was stored
in a room with controlled temperature and relative humidity (20 ±
0.3 °C and 50 ± 3%, respectively) for 14 d. Next, the specimens were
exposed to 5 ± 0.1% carbon dioxide, relative humidity of 60 ± 5%,
and temperature of 23 ± 3 °C in an accelerated carbonation cham-
ber. Carbonation depth was evaluated (using a phenolphthalein pH
indicator) after approximately 76 d of exposure in the accelerated
carbonation chamber.
5.3. Test results and discussion

A ¼ A0 þ St0:5
where A is the water absorption by unit area of concrete surface
from the moment the sample was dipped in water, S is the sorptiv-
ity of the material, t is the elapsed time, and A0 is the water
absorbed initially by pores in contact with water.
ð5Þ Results of fresh SCC testing are presented in Table 12, along
with the consistency classification according to EN 206-9 [64]. As
shown in Fig. 8, all mixtures exhibited good deformability, a uni-
form distribution of aggregates in the spread area, and no signs
of segregation. Based on results of fresh state tests, both SCC-A
and SCC-B belong to SF2 + VS1/VF1 + SR2 consistency classes.

Fig. 9. (a) Evolution of resistivity over time, (b) relation between four-electrode and two-electrode resistivity results (water curing at 20 ± 2 °C until testing age).

Fig. 10. Penetration depth of chloride ions (lighter part, indicated by arrows): (a) SCC-A, (b) SCC-B, and (c) SCC-C.
648 J.P. Moretti et al. / Construction and Building Materials 172 (2018) 635–649
SCC-C exhibited lower deformability and higher viscosity inas-
much as it was classified as SF1 + VS2/VF2 + SR2. When the J-ring
with the highest number of rebars (16) was used, none of the mix-
tures satisfied the EN 206-9 [64] criterion of a J-ring step lower
than 10 mm. Nevertheless, mixtures SCC-A and SCC-B exhibited
J-ring step values closer to 10 mm when compared to SCC-C. This
means that these mixtures might not be adequate for zones with
very high density reinforcement, yet are adequate for most current
applications such as housing construction.
Fig. 9(a) presents the evolution of electrical resistivity measure-
ments with time, obtained with both the two-electrode and four-
electrode methods. As reported before by Silva et al. [65], higher
values of resistivity are obtained when using the four-electrode
method as compared to the two-electrode method, and a good lin-
ear correlation was found between the results of both tests (see
Fig. 9(b)). The average test results of static modulus of elasticity
and compressive strength, at 28 d, are shown in Table 12. In the
case of the SCC-A mixture, compressive strength results are not
presented owing to improper regularisation of the cylinder faces
in contact with the plates of the testing machine, which led to
abnormal results. Based on the average results of compressive
strength at 28 d, SCC-B and SCC-C can be classified as C40 and
C35, respectively, according to EN 1992-1-1 [66]. In addition, one
can expect SCC-A to exhibit a compressive strength greater than
53 MPa; thus, it is classified as C45. Average results from the
migration test carried out on 28 d old SCC specimens, after apply-
ing a voltage of approximately 30 V and 25 V for 24 h on SCC-A and
-B and SCC-C specimens, respectively, are presented in Table 12.
The penetration depth of chlorides obtained after spraying silver
nitrate solution over the split faces of the specimens can be
observed in Fig. 10. Based on chloride diffusion coefficient results,
all three SCC mixtures can be classified as normal quality concrete
according to the classification proposed in [67]. Eq. (5) was found
to provide a very good fit to the data of water absorption by capil-
larity versus t 0:5 , with coefficients of determination (R2) greater
than 0.96. The average sorptivity value of SCC-A, SCC-B, and SCC-
C is 0.356, 0.378, and 0.378, respectively. Thus, SCC-A is expected
to exhibit improved durability when compared to mixes SCC-B
and SCC-C. As anticipated, carbonation depth increased with an
increase of w/c [40].
6. Conclusions
Based on the presented experimental results and statistical
analysis of data, the following conclusions can be drawn:

Replacing cement by up to 30% SBA, in terms of weight, had no
significant effect on mortar fresh state properties or mortar
resistivity at 28 d. SBA/c was found to be significant only for
the compressive strength at 28 d, and yet its effect was rela-
tively small.

The variable w/c had the most significant effect on almost all
the mortar response variables, exceeded only by the effect of
Vw/Vp on Tfunnel and por, 28 d responses.

No significant increase in mortar compressive strength (7–17%)
or mortar resistivity (15–28%) was observed from 28 to 91 d,
which can be attributed to the low pozzolanic activity of SBA.

A number of different mortar compositions were found that sat-
isfy the requirements of self-compactability for different w/c
levels.

Concrete test results revealed that SBA can successfully be used
as a filler material in SCC that exhibits good self-compacting
ability and strength levels, as well as, durability indicators
results adequate for many current civil engineering
applications.
Conflict of interest
None.
Acknowledgements
The authors acknowledge the Erasmus Mundus EBW+ program
for the scholarship; CONSTRUCT/FEUP and LABEST group, engineer
Paula Silva, and Cláudio Ferraz for their support in experimental
tests; CAPES and MCTI/CNPq (grant 309.822/2013-9); the Post-
Graduate Program in Structures and Civil Construction (PPGECIV)
of Federal University of São Carlos (UFSCar); the Institute for Tech-
nological Research of São Paulo (IPT); and Raízen for supplying
SBA.
This work was financially supported by: Project POCI-01-0145-
FEDER-007457-CONSTRUCT-Institute of R&D In Structures and
Construction funded by FEDER funds through COMPETE2020 –
Programa Operacional Competitividade e Internacionalização
(POCI)–and by national funds through FCT–Fundação para Ciência
e a Tecnologia. Collaboration and materials supplied by Concremat,
Secil, Omya Comital, and Sika are gratefully acknowledged.
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