Arabian Journal for Science and Engineering (2022) 47:12873–12887

https://doi.org/10.1007/s13369-022-06641-8

RESEARCH ARTICLE-CIVIL ENGINEERING

Effect of Colemanite Ore Wastes Utilization on Fresh Properties

and Compressive Strength of Cementitious Systems
Süleyman Özen1 · Muhammed Yasin Durgun2 · Veysel Kobya3 · Kemal Karakuzu3 · Ali Mardani-Aghabaglou3

Received: 7 October 2021 / Accepted: 23 January 2022 / Published online: 20 February 2022
© King Fahd University of Petroleum & Minerals 2022

Abstract
In this study, the usability of colemanite wastes (CW), in mortar mixtures, was examined in terms of compressive strength,
while at the same time it was aimed to evaluate the effects of this waste on the rheological properties of mortar and paste
mixtures. Mortar and cement paste mixtures were produced by substituting 1, 3, 5, and 7% of the cement with the CW.
Marsh-funnel flow times, mini-slump values, rheological parameters, and setting times of cement paste mixtures containing
CW were determined. The time-dependent slump-flow and 1-, 7-, 28-, and 56-day compressive strength values of the mortar
mixtures were determined. The microstructures of the specimens were evaluated by using SEM images, and phase analyses
were examined with XRD analysis. The results showed that the use of CW negatively affected the fresh state properties
and rheological parameters of cementitious systems. However, CW addition decreased the 1-, 7-, and 28-day compressive
strength. Only a slight increase was observed in the strength of mixtures containing 5 and 7% CW at 56 days.

Keywords Colemanite wastes · Cementitious systems · Fresh properties · Rheological parameters · Compressive strength

1 Introduction waste materials [5] such as fly ash [6], ground granulated
blast furnace slag [6, 7], silica fume [8], rice husk ash [9],
The greenhouse gasses cause global warming, and it is stated and waste marble dust [10]. Some of these mentioned min-
that the cement industry is responsible for 5–8% of total eral additives such as fly ash and ground granulated blast
anthropogenic CO2 emissions [1, 2]. On the other hand, the furnace slag are major industrial solid wastes. Solid waste
increasing demand for cement production poses a threat to management has gained great tremendous in recent years.
natural sources. The use of mineral additives in cement and The storage and disposal of these industrial solid wastes have
concrete production has become widespread due to the men- become a huge problem [11, 12]. The fact that some parts of
tioned reasons [3, 4]. Most of these mineral additives are these solid wastes can be used in the cement and concrete
industry contributes to the solution of this problem [13].
B Muhammed Yasin Durgun One of these wastes generating industrial facilities is
mydurgun@bartin.edu.tr boron plants. The importance of boron minerals is increas-
Süleyman Özen ing day by day. Boron reserves are concentrated in a few
suleyman.ozen@btu.edu.tr countries in the world. Evaluation of boron waste in the coun-
Veysel Kobya tries having the highest boron reserves in the world such as
v.kobya@gmail.com Turkey, Russia, South America, and the USA is important.
Kemal Karakuzu Turkey has 73.4% of the boron reserves in the world, and
karakuzu.kemal@gmail.com this ratio makes Turkey first in the world. It is estimated that
Ali Mardani-Aghabaglou the world boron production capacity in 2019 is 5.7 million
ali.mardani16@gmail.com tonnes, and the actual world boron production is 3.8 million
1 Department of Civil Engineering, Bursa Technical University, tonnes. Turkey is the first in production with a 56% share
Bursa, Turkey [14]. Boron cannot be found as free in nature. Boron ele-
2 Department of Civil Engineering, Bartın University, Bartın, ments can be found at different amounts in the structure of
Turkey different minerals [15]. There are approximately 230 differ-
3 Department of Civil Engineering, Bursa Uludag University, ent boron minerals in nature. Colemanite is the most common
Bursa, Turkey and commercial boron mineral in Turkey with tincal and ulex-

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ite [16]. The most common method used during the extraction
and processing of boron minerals is the separation of clay in
the boron mineral by using mechanical methods. At the end
of these processes, some wastes containing boron minerals
arise where the clay and boron minerals cannot be separated
from each other [17]. This production creates large amounts
of wastes. These wastes can cause economic and ecologi-
cal problems. The wastes are collected in the pools around
the facilities. If they are directly discharged into the environ-
ment, they have the potential for environmental pollution. In
particular, they pose a threat to underground water resources
[18–20]. For this reason, many studies have been conducted
on the utilization of boron wastes in various fields. Among
these studies, some studies on the use of boron wastes in
cement and concrete production are also observed.
Erdoğan et al. [21] substituted 1, 3, 5, and 7% of cement
with colemanite ore wastes in cement systems and suggested
using up to 5%. Kula et al. [22] used CW up to 9% with coal
bottom ash and fly ash in mortar production. They reported
that using up to 3% of CW improved the mechanical prop-
erties of the 28-day specimens. In another study [23], Kula
also used tincal ore waste (another waste containing boron)
with the same ashes and reported a significant compressive
strength reduction beyond 5%. Targan et al. [24] used 4%
CW in cementitious systems containing different amounts of
bentonite. As a result, they stated that the use of 5% bentonite
in systems containing 4% CW gives strength values compa-
rable to concretes produced with 100% Portland cement. In
another study by the same author, 4% CW was used with dif-
ferent amounts of natural pozzolan in concrete and obtained a
significant compressive strength increase after 28 days [25].
Sevim et al. [26] used CW up to 15% instead of cement in
concrete. They reported higher compressive strength values
at 28, 90, and 180 days by 3% CW addition and similar com-
pressive strength to reference specimen at 180 days by 5%
CW addition. In another study of Sevim, drying shrinkage
of mortar containing CW up to 15% was investigated. It is
reported that CW reduced the drying shrinkage between 7
and 37% [27]. Öztürk and Özdemir [28] used colemanite
wastes with two different B2 O3 ratios (22.48 and 8.23%) up
to 10% in cement systems. It is recommended to use up to
5 or 10% of CW instead of cement since it does not cause a
severe decrease in mechanical properties. In another study,
Mutuk and Mesci [29] investigated the use of CW with rice
husk ash in mortars. In some studies, the use of boron wastes
directly in cement production has been investigated [19, 30].
In addition, in some studies, the contribution of boron miner-
als to radiation shielding properties in cementitious mixtures
has been investigated [31, 32]. In a limited number of studies,
the durability properties [33] and high temperature resistance
of boron minerals in cemented systems [34] have been inves-
tigated. The common finding of the researchers is that the use
of wastes containing boron minerals in cementitious systems
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has an extending effect of setting time [21, 22, 24, 25]. On
the other hand, it is seen that the usability of wastes contain-
ing boron in different applications such as geopolymers and
tiles are investigated [18, 35–37]. However, the effect of CW
on the rheological properties of cement systems is of great
importance due to its effect on the setting time.
Fresh cement paste is a fluid with non-Newtonian behav-
ior. Knowing the rheological properties has great importance
in characterizing the flow of fresh cement paste [38]. The
rheology of cement-based materials in the fresh state is often
expressed by yield stress and plastic viscosity [39]. Roussel
[40] expressed the yield stress as “the minimum stress for
irreversible deformation and flow to occur.” In practice, it
is stated that yield stress is an important parameter related
to filling the formwork. On the other hand, plastic viscosity
is stated to be a term related to pumping ability. The rhe-
ology of fresh cement paste is highly complex because it
is affected by design parameters, chemical and mineralogi-
cal factors, mixing processes, experimental conditions, and
chemical and mineral additives [41]. Generally, it is stated
that the use of mineral additives has a negative effect on
workability in mixtures with a constant solid volume. The
most important reason for that is that the increase in the total
amount of powder in the mixture increases the water demand
due to the rise in the total specific surface area. However, there
are studies in the literature in which exact opposite situations
were observed [42]. Therefore, performing rheological tests
on cement paste is crucial to choose the right type and dosage
of mineral additive and improve concrete workability [43].
As it is known that the importance of boron mines is
increasing day by day, which means wastes containing
boron minerals will be encountered more frequently in the
near future [17]. The use of boron wastes is essential in
terms of economy, recycling, and sustainability in terms of
reducing cement demand and utilizing waste materials in
concrete production. It is also an advantage to be able to
substitute cement with other binders in terms of improving
the mechanical and durability performance of concrete mix-
tures. Turkey, Russia, South America, and the USA are the
countries with the highest boron reserves in the world [14].
For this reason, it is more essential to evaluate boron wastes
in the mentioned countries. There are various studies in the
literature on the use of boron wastes in cement systems.
However, there is still a lack of research in the literature
about the effects of waste containing boron minerals on the
fresh state properties of cementitious systems, especially
on rheological and time-dependent performances. In this
study, the effect of partial replacement of cement with CW
on flowability, setting time, and rheological properties of
cement paste, and the time-dependent fresh state behavior of
mortar mixtures were investigated. Besides, the compressive
strengths of the mortar mixtures were determined. SEM
Arabian Journal for Science and Engineering (2022) 47:12873–12887 12875

micrographs were taken, and XRD analysis was performed 5

to examine the microstructure of the mortar mixture.

2 Materials and Method

Intensity
2.1 Materials

In this study, CEM I 42.5-type Portland cement was used in

accordance with TS EN 196-1. Cement was partially replaced 4
1
5 2
1,5 3
5
1 3
with CW supplied from Bigadiç/Balıkesir in different pro- 2 1 6 11
5
2
5 2
2 52
portions. The chemical component, physical and mechanical
properties of cement and CW supplied by the manufacturer
10 20 30 40 50 60 70
are given in Table 1. The mean size of cement and CW is
2θ
32 and 47.9 μm, respectively. Also, the results of the XRD
analysis and the SEM image of the CW are shown in Figs. 1 Fig. 1 XRD patterns of CW. 1: colemanite, 2: feldspar, 3: mullite, 4:
and 2, respectively. illite, 5: calcite, 6: kaolinite
Significant borate deposits in the world have formed as
evaporates sandwiched between non-marine clay and lime- respectively, according to the TS EN 1097-6. Sieve analysis
stone layers. Fluids with high boron content are transported of aggregate is shown in Table 2. Polycarboxylate ether-based
by volcanic sources to the location of the deposits, and the high-range water-reducing admixture was used to achieve
dissolved boron begins to precipitate here due to evapora- the desired flow value in the mixtures. Some properties of
tion. After boron is deposited here, it remains under a layer the water-reducing admixture given by the manufacturer are
of clay and limestone deposits and settles in the geologi- summarized in Table 3.
cal environment. Therefore, clay impurities are frequently
encountered in boron mines [44]. As seen in Fig. 1, CW 2.2 Preparation of Mixtures
contains aluminum, silicate, and calcium phases as well as
colemanite. Simultaneously, the presence of illite and kaoli- It was emphasized in the literature that the wastes contain-
nite, two important clay groups were also observed. ing boron minerals affect the setting time of cementitious
In the scope of the study, crushed limestone aggregate mixtures negatively. For this reason, it was recommended
with a maximum grain size of 5 mm was used in accordance that the CW should be used below 10% in cementitious sys-
with TS EN 206-1. The specific gravity and water absorption tems [21, 28, 45, 46]. In this context, in the mixtures prepared
capacity of the aggregate were determined as 2.65 and 2.03%, within the scope of the study, in addition to the control mix-

Table 1 Physical, chemical, and mechanical properties of binders

Oxides (%) Cement CW Mechanical properties Cement CW

B2 O3 – 14.20 Compressive strength (MPa) 1-dayb 14.7 –

SiO2 18.86 16.83 2-dayb 26.8 –
Al2 O3 5.71 1.28 7-day 49.8 –
Fe2 O3 3.09 0.262 28-dayb 58.5 –
CaO 62.7 25.60 Physical Properties
MgO 1.16 13.43 Specific gravity 3.15 2.42
a SO 2.39 0.34 Residual on 32μm sieve (%) 19.9 21.66ô
3
Na2 O + 0.658 K2 O 0.92 0.11 Residual on 45μm sieve (%) 4.3 14.19
a Cl− 0.01 – Residual on 90μm sieve (%) 0.2 5.02
Insoluble residue kalıntı 0.32 –
Loss on ignition 3.2 16.83
Free CaO 1.26 –
a According to TS EN 197, SO3 ≤ 3.5% and Cl- ≤ 0.01
b According to TS EN 197-1, CEM I 42.5-type cement should have the 2-day compressive strength ≥ 20 MPa and the 28-day compressive
strength ≥ 42.5 MPa

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concrete is produced [47]. It has been stated that the higher the
CPV, the higher the flowability of the fresh mixture [48]. In
this study, it can be seen that there is no significant change in
the CPVs of the mixtures and it is kept as constant as possible.

2.3 Experimental Method

The effect of CW substitution on fresh state, rheological

properties, and compressive strength in cementitious sys-
tems was investigated. For this purpose, paste and mortar
mixtures were prepared as the control without CW, and CW
substituted in four different ratios (1, 3, 5, 7%). In each
paste mixture, Marsh-funnel flow time, mini-slump, rheolog-
ical properties (static and dynamic yield stress, viscosity),
Fig. 2 SEM image of CW setting time experiments were performed. In each mortar
mixture, admixture requirements for target slump-flow value
Table 2 The particle size distribution of aggregate used in mixtures (220 ± 10 mm), consistency retention performance, and com-
Sieve size (mm) Passing (%) Residual (%) pressive strength were investigated.
Marsh-funnel and mini-slump tests were carried out to
5.60 100 0.00 determine the workability properties of paste mixtures. The
4.00 99.20 0.80 water/binder ratio was kept constant at 0.35 in all cement
2.00 76.45 23.55 pastes [49, 50]. Setting time of the mixtures was determined
1.00 52.33 47.67 by using an automatic Vicat apparatus according to TS EN
0.50 31.65 68.35 196-3.
0.25 19.18 80.82 A rheometer with a ball measuring system (BMS) shown
0.125 3.91 96.09 in Fig. 3a was used to determine the rheological properties
of cement pastes. The maximum shear rate, maximum
moment, and maximum shear stress values of the rheome-
ture that does not contain CW, five different cement paste and ter are 35 s−1 , 200 mN.m, and 4560 Pa, respectively. In
mortar mixtures were prepared by replacing 1, 3, 5, and 7% rheological measurements, the 4-period method suggested
of cement with CW. The mixtures were designated accord- by Mardani-Aghabaglou et al. [51–53] was applied and is
ing to the CW replacement ratio. For example, the control shown in Fig. 3b.
mixture which does not contain CW was shown as C, and Rheological properties of the mixtures were obtained
the mixture in which 1% of cement was substituted by CW statically and dynamically. To obtain the static yield stress,
was indicated as CW1. first-period measurements shown in Fig. 3b were taken into
Water/binder, sand/binder ratio, and slump-flow values for account. For this purpose, the shear stress–time diagram
all mortar mixtures were kept constant in accordance with of the mixtures for the first period was plotted and the
ASTM C109 as 0.485, 2.75, and 220 ± 20 mm, respectively. maximum shear stress value was determined as the static
Different ratios of water-reducing admixture were used to yield stress of the mixtures. The static yield stress value
provide the desired slump-flow value in the mixtures accord- represents the measurement obtained without any process
ing to the total binder weight. The amount of materials used after the mixture’s preparation. In measuring the dynamic
in the preparation of the mortar mixtures are shown in Table yield stress and viscosity of the mixture, fourth-period
4. Table 4 also gives the volume of cementitious paste volume values were taken into account. For this purpose, the shear
(CPV) of the mixtures. In the literature, it has been stated that stress/viscosity–shear rate diagrams of the mixtures were
voids between the aggregate particles cannot be sufficiently obtained. The point where the shear stress curve intersects
filled by a lower amount of CPV. Therefore, more permeable the shear axis was determined as the dynamic yield stress of

Table 3 Properties of
water-reducing admixture Type Density (g/cm3 ) pH value Chloride content (%) Alkaline content Na2 O
(%)

Polycarboxylate 1.023–1.063 5–8 <0.1 <10

ether-based

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Table 4 Mixture design of mortars

Cement (g) CW (g) Water (g) Aggregate (0–5 mm, g) HRWRA (%)* Slump-flow value (mm) Cementitious paste
volume (%)

C 500 0 242.5 1375 0.44 23.0 43.73

CW1 495 5 242.5 1375 0.50 22.3 43.78
CW3 485 15 242.5 1375 0.70 23.0 43.90
CW5 475 25 242.5 1375 0.86 22.2 44.00
CW7 465 35 242.5 1375 1.10 22.1 44.13
*High-range water-reducing admixture

Fig. 3 a Rheometer device, b methods applied in rheological measurements [51–53]

the mixture. The last constant value of the viscosity curve is
taken as the apparent viscosity value of the mixture.
The slump-flow performance of the mortar mixtures was
determined according to the ASTM C1437. The specimens
were prepared to determine the compressive strength of mor-
tar mixtures in accordance with ASTM C109 and removed
from the molds 24 h after casting. They were cured in lime-
saturated water at 23 ± 2 °C until the test day in conformity
with ASTM C511. The 1-, 7-, 28-, and 56-day compressive
strengths of the mortar specimens were determined on 50-
mm cube specimens according to the ASTM C109.
3 Result and Discussion
3.1 Fresh State Properties
3.1.1 Marsh-Funnel Flow Time and Mini Slump
The process of the experiments and Marsh-funnel flow times
of cement paste mixtures are shown in Fig. 4. As expected,
Marsh-funnel flow time of mixtures reduced with the increase
in the admixture dosage. In the case that water-reducing
admixture less than 1% was used, the measurement could
not have been taken because the control and CW1 mixtures
did not flow through the Marsh funnel. A similar situation
is observed when the amount of water-reducing admixture
in CW3, CW5, and CW7 mixtures is below 1.25, 1.75, and
1.75%, respectively. The flow performance of the mixtures
was adversely affected by the use of CW and the increase
in the usage ratio. For example, when the use of admixture
was 2%, the increase in Marsh-funnel flow time of CW1,
CW3, and CW5 existed by 2, 4 and 10% compared to the
control mixture, respectively. This increase was 77% for the
CW7. It is understood from Fig. 4 that the saturation points
of the water-reducing admixture in mixtures containing 0,
1, 3, 5, and 7% CW are 1.25, 1.5, 1.75, and 2%. As seen
from the results, the need for water-reducing admixture to
reach saturation of the paste mixtures increased with the rise
of CW content in the mixtures. No significant change was
observed in the flow times of the mixtures beyond the satu-

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Fig. 4 a Preparation of the

mixture b performing of flow
time, c performing of mini
slump, d measurement of
mini-slump value,
e Marsh-funnel flow times of
paste mixtures

(a) (b)

(c) (d)
50
C CW1 CW3 CW5 CW7
Marsh funnel flow time (s)

40 Saturation point

Saturation point
Saturation point
30

20
1 1.25 1.5 1.75 2 2.25 2.5
Admixture/Cement (%)
(e)

ration point. In this context, the admixture saturation point is
economically essential [52, 53].
Mini slump and temperatures of cement paste mixtures
are given in Table 5. Regardless of the CW in the mixtures,
it was observed that the mini-slump values of the mixtures
increased with the rise of the admixture content. The sub-
stitution of CW in the paste mixtures negatively affected
the consistency of the mixtures as in the marsh-funnel flow
test. The reduction in the mini slump was observed with the
increase in CW at the same admixture ratios. The addition
of admixtures into the mixtures beyond the saturation point
did not significantly affect the mini-slump values similar to
the Marsh-funnel flow test.

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Table 5 Mini slump and

temperature of pastes Admixture/cement ratio (by 0.75 1.00 1.25 1.50 1.75 2.00 2.25
weight %)

Mini slump (mm) C 125 217 230 231 234 235 235
CW1 114 189 198 201 205 205 206
CW3 109 119 195 201 202 203 202
CW5 No flow 83 103 167 192 195 195
CW7 No flow No flow 98 109 155 159 158
Temperature (°C) C 27.2 27.4 27.6 27.5 26.5 26.1 26.3
CW1 29.6 29.0 28.8 28.4 28.1 27.8 27.7
CW3 29.2 28.3 27.8 27.4 26.6 26.3 26.3
CW5 28.9 28.7 28.7 28.5 28.2 27.9 27.8
CW7 28.7 28.6 28.4 28.2 27.9 27.9 27.8

It was observed that the temperature of the mixtures
decreased by 1–2° as the dosage of water-reducing admix-
ture increased in the paste mixtures. It is thought that this
decrease is due to the low set retarding effect of CW and
water-reducing admixture.
According to the literature, the use of boron in cemen-
titious systems negatively affected the consistency retention
properties of the mixtures. It increased the need for admixture
for constant consistency [54]. Gencel et al. [55] stated that
the slump values decreased with the increase in colemanite
content in concrete mixtures. They claimed that this nega-
tive effect resulted from colemanite causing agglomeration
in concrete mixtures.
3.1.2 Rheological Parameters
The shear stress–time graph of the mixture is drawn in Fig. 5
by taking into account the data obtained from the first period
to obtain the static shear stress of the mixtures. The maxi-
mum value of shear stress on the curve was chosen as the
value of static shear stress of the mixture (undisturbed). To
obtain the dynamic rheological parameters of the mixtures,
the shear stress/viscosity–shear rate graph was obtained by
taking into account the measurements in the fourth period
for each mixture (Fig. 6). The values of dynamic shear
stress and final viscosity obtained from the curves accord-
ing to the “Herschel–Bulkley” model are given in Table 6.
As seen from Fig. 6, the experimental shear stress and
shear rate relationships are in good agreement with the Her-
schel–Bulkley model. The equation of Herschel–Bulkley
model is given below;
τ  τ0 + a × γ̇ b
where a is the consistency coefficient of Herschel–Bulkley
model and b is called Herschel Bulkley index. The Her-
schel–Bulkley model may be concave upward or downward
related to the value of b. When the exponent b is set to less
than unity, the curve will be concave downward and this
behavior is named shear-thinning or the pseudoplastic. When
the exponent b is set to larger than unity, this curve will be
concave upward and this flow is called shear-thickening or
dilatant [56]. In Fig. 6, all the curves of Herschel–Bulkley
are concave downward and this indicates that all mixtures
represent the pseudoplastic flow. In fact, it is known that
the boron minerals and the wastes containing boron miner-
als slow down the hydration process due to the precipitated
compounds (calcium borate (CaO.B2 O3 )) on cement grains
[57]. Due to this situation, it was expected that the worka-
bility would be higher and maintained for a longer period
as an effect of slowing hydration. However, irrespective of
static and dynamic behavior, yield stresses of the mixtures
increased with the increase in CW utilization level. Similar
results were obtained for final viscosity. This behavior was
more pronounced in the case of high CW containing. This
phenomenon is thought to be since CW waste contains clay
and its loss of ignition is high. According to Fig. 1, the CW
wastes used in this study include clay derivatives such as illite
and kaolinite. It is known that clay minerals absorb the water
in their layered structure and increase the water demand [58].
Similar results regarding the negative effect of clay content
on cementitious systems were reported by other researchers
[45, 46].
According to Table 1, the loss of ignition value for CW
used in this study was obtained as 16.83%. Sevim et al. [26]
reported a workability reduction by the use of CW. They
thought the reason for the workability loss is the high loss
on ignition of CW. Phenthany [59] reported that an increase
in loss on ignition increases the water-retaining property of
the mixture which causes lowering the free water content
(1) and resulting in a decrease in the slump of the cementitious
mixture.

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Fig. 5 Time-dependent shear
stress change of (Period 1)
Fig. 6 Shear stress–viscosity and shear rate relation
3.1.3 Setting Time
The initial and final setting times of the paste mixtures are
shown in Table 7. The replacement of cement with CW
caused the initial and final setting time of cement paste mix-
tures to be prolonged. This effect was more pronounced with
the increase in the CW substitution ratio. The initial and final
setting times were delayed up to 40 and 60% with the increase
in the amount of CW, respectively. Especially, using more
than 5% of the CW amount led to a significant increase in the
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Arabian Journal for Science and Engineering (2022) 47:12873–12887
initial and final setting times. Similar results were expressed
by other researchers [16, 21–25, 33, 44, 46, 54, 57, 60–65].
It was reported that the retarding effect of the set-
ting is due to B2 O3 in CW. It was reported that the
setting time of cementitious systems is prolonged due
to the formation of boro-ettringite or amorphous calcium
borate hydrate components during cement hydration [45,
66, 67]. Calcium borate (CaO.B2 O3 ) is formed by the
reaction of boron oxide (B2 O3 ) and calcium hydroxide
(Ca(OH)2 ) during the interaction of cement with mixing
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Table 6 Rheological results of

paste mixtures C CW1 CW3 CW5 CW7

Yield stress (Pa) Static 16.20 21.86 67.99 310.58 672.58

Dynamic 5.49 11.27 61.98 123.85 175.99
Final viscosity (Pa.s) 2.30 3.89 9.06 10.33 13.63

Table 7 Setting time of paste mixtures containing different amount of ratio, the slump-flow loss of the mixtures was more pro-
CW nounced. In mixtures containing CW, the slump-flow loss
Mixture Setting time at the end of the first 15 min was measured between 7 and
15%, while it was found to be between 20 and 28% at the
Initial (min.) Final (min.)
end of 60 min. It was observed that the mixtures showing
C 189 274 the best and the lowest performance at the end of 60 min
CW1 216 301 in terms of consistency retention were control and CW7,
CW3 219 349 respectively. As mentioned before, the setting time of mix-
CW5 221 377 tures is expected to increase with the use of CW. Besides,
CW7 263 438 the required water-reducing admixture increased due to the
rising of the CW content to achieve the desired slump-
flow value. Considering the retarding effect of admixture,
water. This compound partially or entirely covers the sur- it was explained that the consistency retention performance
face of cement particles. Thus, it causes prolongation of of mixtures was negatively affected by the increase in the
setting time by preventing the cement contact with water admixture utilization ratio, contrary to expectations. Since
[57]. It was also declared that the CW having the high the calcium borate formed in mixtures containing CW cov-
loss on ignition might create a delay effect on setting time ers the cement surface, it is thought that the water-reducing
[45]. admixture adsorbs less on the grains. Thus, the amount
of non-adsorbed admixture in the solution is expected to
increase. It is believed that the non-adsorbed admixture is
3.1.4 Time-Dependent Behaviors of the Mortar Mixtures trapped by boro-ettringite and hydrated calcium borate prod-
ucts and thus, the effectiveness of admixture is reduced.
The required water-reducing admixture to provide the desired Besides, as highlighted before, CW contains different types
slump-flow value in mortar mixtures and the time-dependent of clay (Fig. 1). The presence of clay in the mixture decreases
slump-flow value of the mixtures is given in Table 8. The the effectiveness of the water-reducing admixture as well [69,
test procedure is depicted in Fig. 7. With the use of CW, 70].
water-reducing admixture requirement increased to achieve
the desired slump-flow value (220 ± 10 mm) in mortar mix-
tures. This effect was more pronounced with the increase in 3.2 Compressive Strength
the CW ratio. It was emphasized that this effect is because of
the clay content in CW and the high loss on ignition [26, 45, The compressive strengths of mortar mixtures in age 1, 7, 28,
58, 59, 68]. The slump-flow values of the mortar mixtures and 56 days are shown in Fig. 9. As expected, the compres-
decreased by elapsed time, regardless of the CW utilization sive strength of mortar mixtures increased by elapsed time,
ratio. regardless of the CW content.
The time-dependent relative slump-flow values of the mix- The 1-day compressive strength of the mortar mix-
tures are shown in Fig. 8. With the increasing CW substitution tures was adversely affected by replacing cement with

Table 8 Time-dependent flow

value of mortar mixtures Mixture Admixture dosage (%) Time-dependent flow value (mm)

0 min 15 min 30 min 45 min 60 min

C 0.44 23 215 205 191 186

CW1 0.50 223 204 196 183 176
CW3 0.70 23 207 197 185 176
CW5 0.86 222 195 184 174 164
CW7 1.10 221 188 180 170 160

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12882 Arabian Journal for Science and Engineering (2022) 47:12873–12887

Fig. 7 a Performing of
slump-flow test, b measurement
of slump-flow value

C CW1 CW3 CW5 CW7 ative effect arises from the fact that the calcium borate
100
component formed in the mixture slows down hydration
Relative slump-flow (%)

reactions and extends the setting time [71]. Because of

90 the delay in forming C–S–H gels in cementitious systems,
the development of compressive strength also slows down
[64].
80 As shown in Fig. 9, the 56-day compressive strength
of the mixtures containing a higher CW ratio was higher
70
than the control mixture. Similar results were reported by
0 15 30 45 60 other researchers [26, 27, 30, 72]. Compared to the control
Time (min.) mixture, the 56-day compressive strength of the mixtures
containing 5 and 7% CW was slightly higher. This situa-
Fig. 8 Time-dependent relative slump flow of mortar mixtures contain-
ing 0, 1, 3, 5, and 7% of CW tion is thought to be due to the denser microstructure of
the CW in cementitious systems. Similar expressions were
declared by Sevim [27]. It is thought that the mixtures
80
C CW1 CW3 CW5 CW7 containing CW have more regular and non-void structures
70
Compressive strength (MPa)

because of the slow hydration process. According to Olgun

60 et al. [73], microstructure development delays because of the
50 delay setting time in mixtures containing CW and needle-
40 like hydration products (boro-ettringite) are formed. In the
30
microstructure analysis performed within the scope of the
study, it was understood that the boro-ettringite structure
20
formed in the mixtures containing CW (Fig. 10). The pres-
10 ence of boron minerals in CW structure causes a stronger
0 bond between particles due to the denser microstructure [24,
1-Day 7-Day 28-Day 56-Day
66, 74, 75].
Fig. 9 1-, 7-, 28-, and 56-day compressive strength of mortars

3.3 Microstructural and Mineralogical Investigations

CW. 10% reduction in the 1-day compressive strength
was measured with an increase in CW replacement ratio
up to 3% in the mixtures. The increase in CW content
up to 5 and 7% caused a decrease of 22 and 28% in
the 1-day compressive strength of the mixtures, respec-
tively. The negative impact of using CW on compressive
strength was decreased by elapsed time. Similar results
were reported by other researchers [33, 64, 65]. This neg-
The 56-day specimens of control and mixtures containing 1
and 7% CW were used for microstructural analysis. SEM and
XRD analyses were performed on the prepared specimens.
XRD analyses of control, CW1, and CW7 specimens are
given in Fig. 11.
As seen from Fig. 11, there was no significant change
in the XRD pattern due to the small amount of CW in the

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Arabian Journal for Science and Engineering (2022) 47:12873–12887 12883

Fig. 10 SEM images of

ettringite in CW containing
matrices

Ettringite Ettringite

Ettringite
Gypsum

4 C In some studies, ettringite formations were reported in the

CW1
CW7 C–S–H structure in specimens containing CW or coleman-
1,2
2,4,5
ite [72]. On the other hand, some researchers [15, 29, 73]
3 3
3 1 3,4 3,4,5 3 3 3,4 3 reported that they encountered some needle-like hydration
4
products due to the CW usage in SEM analyses. When the
CH crystals detected in the images were examined, it was
Intensity

1,2
observed that the typical hexagonal structure of these crys-
2,4,5
3
3
1 3 3,4 3,4,5 3 3 3,4 3 tals was disrupted. It was stated by Kavas et al. [65], where the
4 morphology of portlandite crystals may be different slightly
in pastes containing CW. This may be due to the increase in
1
portlandite solubility as the boron content increases in the
3
1
3 3,4 3,4 3
3 4
3 3,4
mixture [77].
3
Two SEM images for each mixture, the one from the
10 20 30 40 50 60 70
matrix and the other from the aggregate-paste interface, are
given in Fig. 13.
2θ
When examining the images of the control specimen
Fig. 11 XRD Patterns of C, CW1, and CW7 (Fig. 13a), a quite dense and uniform microstructure was
observed due to the tight clustering of the C–S–H gels. Matrix
structures of CW1 and CW3 specimens (Fig. 13b and c) have
system. In the case that 2θ was 18°, it was observed that CH a different structure compared to the control specimens. It
formed in the control mixture (Fig. 12). was also found that a more porous structure formed and ITZ
In mixtures containing CW, when 2θ was 18°, both CH is more pronounced in these mixtures. However, in the CW5
and boro-ettringite formation were found (Fig. 10). A calcite and CW7 specimens (Fig. 13d and e), a denser and more
peak was observed in all three specimens. It is known that homogeneous microstructure can be seen similar to the con-
the tobermorite (C–S–H) gel phases forming the matrix phase trol mixture. It was understood that the ITZ phase became
of concrete in XRD analysis generally correspond to peaks stronger (more uncertain) with the increase in CW content.
around 28–30° (2θ) [76]. In this study, C–S–H gel phases Similar results were found by Kavas et al. [65] and Mutuk
were found when 2θ was 29.5°. and Mesci [29].

Fig. 12 SEM images of the

control (C) specimen

CH
CH

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12884 Arabian Journal for Science and Engineering (2022) 47:12873–12887

Fig. 13 SEM images of a C,

b CW1, c CW3, d CW5, e CW7 (a) (a)
Matrix

Aggregate

(b) Aggregate
(b)

Matrix

(c) (c) Aggregate

Matrix

(d) Matrix (d)

Aggregate

Aggregate
Matrix

(e) (e)
Aggregate
Aggregate
Matrix
Matrix

123
Arabian Journal for Science and Engineering (2022) 47:12873–12887
4 Conclusions
For the materials used and test methods applied, the following
conclusions can be drawn:
• Substitution of CW in cement paste mixtures negatively
affected Marsh-funnel flow and mini-slump performance.
The admixture demand for the saturation point of the
paste mixture increased with the increase in the ratio of
substitution. Also, the utilization of CW in mortar mix-
tures increased the admixture demand for providing the
target slump-flow value. Besides, time-dependent slump-
flow performance was negatively affected by the increase
in colemanite content of mortar mixtures.
• In terms of rheological properties, the increase was
observed in all three of the viscosity, static and dynamic
shear stress values with the use of CW. This increment
became more pronounced, especially with the use of high
ratios of CW. It is thought that this negative effect is caused
by the high loss on ignition of CW and the clay minerals
in it. In addition, the results obtained from the rheological
tests indicate that the amount of water-reducing admixture
should be increased with the CW to provide acceptable
flow properties.
• An increase in setting times was detected with the increase
in CW amount. This setting delay is due to the B2 O3
component in the CW. It is also thought that the calcium
borate formed as a result of the reaction of B2 O3 covers the
cement particle surface and delays hydration mechanisms.
• The 1-day compressive strength of the mortar specimens
containing CW decreased compared to the control mixture.
This situation is due to the prolongation of hydration and
setting times of boron components in the mixture. How-
ever, this negative effect gradually decreased. The boron
components strengthened the bond between the particles
by improving the microstructure. Therefore, the 56-day
compressive strength of the mortar specimens increased.
• As a result of the XRD analysis, it was observed that the
diffraction patterns of the control specimen and the spec-
imens containing CW were very similar, and generally
similar phases formed. In SEM imaging, it was observed
that the matrix structures of the specimens using 1 and 3%
CW were different from the other specimens and contained
voids between the C–S–H gels.
Acknowledgements The authors would like to thank for their kind
assistance to Eti Mine Works in providing the colemanite waste, Polisan
Construction Chemicals Company in providing the water-reducing
admixture, Polyfibers Company in providing the polypropylene fiber,
and Bursa Cement Factory determining the chemical composition and
physical properties of cement. In addition, the third and fourth authors
acknowledge the scholarship provided by the Turkish council of higher
education (YÖK 100/2000 Program) during their Ph.D. study.
12885
Data Availability All data, models, and code generated or used during
the study appear in the article.
Declarations
Conflict of interest The authors declare that they have no conflict of
interest.
Ethical Approval This article does not contain any studies with human
participants or animals performed by any of the authors.
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