sustainability

Article
Evaluation of the Improvement Effect of Limestone
Powder Waste in the Stabilization of Swelling
Clayey Soil
José Luis Pastor * , Roberto Tomás , Miguel Cano , Adrián Riquelme and Erick Gutiérrez
Department of Civil Engineering, University of Alicante (Spain), 03690 San Vicente del Raspeig, Spain;
roberto.tomas@ua.es (R.T.); miguel.cano@ua.es (M.C.); ariquelme@ua.es (A.R.); egv.mkz@gmail.com (E.G.)
* Correspondence: joseluis.pastor@ua.es; Tel.: +34-965-90-3400 (ext. 1167)




Received: 19 December 2018; Accepted: 24 January 2019; Published: 28 January 2019


Abstract: The natural stone industry generates large amounts of industrial waste every year.
Limestone powder produced by the activity of this industry is dumped into landfills, generating an
environmental impact that could be reduced by using this waste as a binder in building materials.
In the present work, the use of this by-product as an addition for soil improvement of clayey soils has
been studied. The tested natural soil is a soft clay from southeastern Spain, which has been mixed by
adding 5, 10, 15, 20, and 25% of dry limestone dust by total dry weight of the soil. The natural soil and
the additive have been characterized, in addition to the common geotechnical tests, by means of X-Ray
diffraction and X-Ray Fluorescence. The improvement of the geotechnical properties of the mixed
soil has been evaluated by means of the change in the Atterberg limits, free swell index, unconfined
compressive strength, and one-dimensional consolidation test. The change in the microstructure of
the mixed soil has been studied by scanning electron microscopy. In general, the results obtained
show an increase in the strength of the soil and a reduction of its deformability when limestone
powder is added.

Keywords: clay; limestone waste; soil improvement; strength; deformation

1. Introduction
Soil improvement technique has been widely used to reduce soil deformability and increase the
shear strength of soft soils. The most common binders used to stabilize soils are cement and lime, or a
mixture of both. Nevertheless, these binders have high CO2 emissions and use vast amounts of raw
material during their manufacturing process [1]. In this sense, the use of industrial by-products has
two positive environmental effects. On the one hand, it avoids the use of traditional binders, such as
cement or lime, which have a negative environmental effect. On the other, it avoids dumping of the
waste in a landfill, which presents a strong environmental impact.
In recent years, some research has been done to study the effect of using alternative binders for
soil improvement. In this sense, ground granulated blast furnace slag has become one of the most used
binders for this purpose, having shown very good effects, such as reduction of swelling potential [2,3]
and an increase of the shear strength of soils [3–5]. Similar positive effects have been proven when
fly ash is used in clays [6,7]. Kolay and Ramesh [8] found a reduction of the Atterberg limits and
swelling when fly ash was added to clayey soils. Horpibulsuk et al. [9] also reported a strength increase
of clayey soils when using fly ash as a binder [10], with similar results to those obtained by other
researchers [11–13]. The type of available industrial waste depends on the kind of industrial activity
in an area or country. Therefore, new binders are being tested to know the effect of its addition to
different soils. For example, rice husk ash is one of these new binders that are being used. The general

Sustainability 2019, 11, 679; doi:10.3390/su11030679 www.mdpi.com/journal/sustainability

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of its addition to different soils. For example, rice husk ash is one of these new binders that are being
effect
used.of thisgeneral
The ash consists
effect of
of an
thisincrease in the of
ash consists unconfined
an increase compressive strengthcompressive
in the unconfined and a decrease in the
strength
swelling pressure [6,14,15]. Also, bagasse ash is being studied as a potential addition
and a decrease in the swelling pressure [6,14,15]. Also, bagasse ash is being studied as a potential to expansive
soils. Hasan
addition et al. [16] found
to expansive that this
soils. Hasan etadditive has a modest
al. [16] found that thiseffect on soil
additive hasstrength
a modest buteffect
significantly
on soil
reduces the shrink-swell capacity of expansive clays.
strength but significantly reduces the shrink-swell capacity of expansive clays.
Spain
Spainisisthe
the7th largest stone
7th largest stone producer
producer in in the
the world,
world, having
having aa natural
natural stone
stone production
production of of 3.49
3.49 Mt
Mt
in
in2015
2015[17].
[17]. The
The natural
natural stone
stone industry
industry isis one
one ofof the
the most important economic
most important economic activities
activities in
in southeast
southeast
Spain. Consequently, a huge amount of industrial waste is produced every year
Spain. Consequently, a huge amount of industrial waste is produced every year by this activity. by this activity. This
Thisis
is not
not a concern
a concern only
only for for Spain;
Spain; for for example,
example, up up to 345,000
to 345,000 tonstons of natural
of natural stone
stone sludge
sludge is produced
is produced per
per year at the European-wide level [18]. Much of this waste is landfilled, resulting in an
year at the European-wide level [18]. Much of this waste is landfilled, resulting in an environmental
environmental
impact. Figure 1impact.
showsFigure
a series1 shows a series of
of unplanned unplanned
landfills landfillsprovince
in Alicante in Alicante
(SE,province
Spain) with(SE, Spain)
a clear
with a clear
impact on theimpact on the landscape.
landscape.

Figure 1.
Figure 1. View
View of
of natural
natural stone
stone waste
waste landfills
landfills (LW)
(LW) in
in Alicante
Alicante province
province (Spain).
(Spain).

Efforts are
Efforts are being
being made
madetotofind findanyany useuseforfor
thisthis
waste which
waste avoids
which putting
avoids it intoitlandfills.
putting Since
into landfills.
this isthis
Since a global problem,
is a global some research
problem, some research has been hasdone
beenlately
donein different
lately countries
in different to use the
countries to marble
use the
waste powder
marble waste powderas a mix as awith different
mix with materials.
different OneOne
materials. of the principal
of the principal uses
uses hashasbeen
beenasasaa partial
partial
replacementof
replacement ofcement
cement for for mortar
mortar andand concrete
concrete [19–22].
[19–22]. Some
Some workwork has has also
also been
been done
done to to investigate
investigate
thepotential
the potential of of the
the marble
marble dustdust for
for being
being usedused as as aa binder
binder for for soil
soil improvement.
improvement. AlthoughAlthough therethere is is
stillmuch
still muchresearch
researchto to be
be done
done to to better
better understand
understand the the effects
effects ofof marble
marble dust
dustpowder
powderfor forthis
thispurpose,
purpose,
somepromising
some promisingresults resultshavehavebeenbeen produced
produced by former
by former works.works.
Sivrikaya Sivrikaya et reported
et al. [23] al. [23] reported
a reduction a
reduction
of of the limits
the Atterberg Atterberg
andlimits and anin
an increase increase in the maximum
the maximum dry unit dry unitwhen
weight weight when and
marble marble and
granite
granite powder
powder from stone from stonewere
plants plants were to
added added to artificial
artificial clayeySaygili
clayey soils. soils. Saygili [24] found
[24] found a reduction
a reduction in the
in the
free freeindex
swell swellandindexan and an increase
increase in the unconfined
in the unconfined compressive compressive
strengthstrength
and in the andinternal
in the internal
friction
friction
angle angle
when whendust
marble marblewasdustaddedwastoadded
a clayey to asoil.
clayey soil. Similar
Similar results
results were were obtained
obtained by Sabat byetSabat et
al. [25],
al. [25],
who who reported
reported an increase an increase in the strength
in the strength of the soil ofby
themeans
soil byofmeans of unconfined
unconfined compressive compressive
strength
strength
and and the California
the California Bearing RatioBearing Ratio
tests. Thistests. This
raise wasraise was recorded
recorded for marble for marble dust addition
dust addition up to 20% up
to 20% by dry weight of soil. When this percentage was increased, a
by dry weight of soil. When this percentage was increased, a reduction of the strength was reported. reduction of the strength was
reported. the
However, However,
swelling thepressure
swelling pressure when
decreased decreasedmarblewhen
dustmarble dust was
was added up toadded up to a percentage
a maximum maximum
percentage
used of 25% used of 25%
of marble of marble
dust. The same dust. The same
behavior behavior
of the expansive of the expansive
index index was
was observed observed
by Ali by
et al. [26].
Ali et al. [26]. Sol-Sánchez et al. [27] found that dolomitic lime from residual
Sol-Sánchez et al. [27] found that dolomitic lime from residual sludge was effective as a stabilizing sludge was effective as
a stabilizing
addition addition
to clayey andtomarly
clayey anddue
soils marly soils
to the due to in
increase thepH increase
values,incarbonate
pH values, carbonate
content, andcontent,
particle
anddistribution
size particle sizeofdistribution
the mixed soil of when
the mixed soil when
this binder this binder
was added. was et
Sivrikaya added.
al. [23]Sivrikaya
reported et al. [23]
a decrease
reported a decrease in Atterberg limits and an increase in
in Atterberg limits and an increase in the maximum dry unit weight of the compacted mixedthe maximum dry unit weight of soil
the
compacted
when marblemixedwastesoil whenwas
powder marble
added wasteto anpowder was
artificial added
clayey to an
soil. artificial
Also, clayeyinsoil.
an increase the Also,
strengthan
increase in the strength properties of the mixed soil was found by Brooks
properties of the mixed soil was found by Brooks et al. [28] when limestone dust was added, although et al. [28] when limestone
dust was added, although this increase was not as high as reported in other works for marble dust.
Sustainability 2019, 11, 679 3 of 14

this increase was not as high as reported in other works for marble dust. Ogila [29] found a reduction
in the swelling characteristics of high expansive soil when the limestone dust was mixed with the soil.
Sabat and Muni [30] also reported an increase in the strength properties of clayey soils when limestone
dust was added. Moreover, a decrease in the liquid limit and the plasticity index and an increase in the
plastic limit was found. Nevertheless, according to Brooks et al. [28], there are a limited number of
studies about the possible utilization of limestone powder in construction.
Other researchers have studied the stabilization of effluent-contaminated cohesive soils using
industrial by-products, such as marble dust and ground granulated blast furnace slag [31], although in
this case, the industrial leachate prevents the addition from having the expected positive results.
In this work, the effect of adding limestone powder waste to a clayey soil was studied. The soil
used for this work is a natural soil obtained from a trench in a construction site, instead of a clay made
with the combination of different clay mixtures, which is more common in the literature. The present
work broadens the knowledge of the effect of this by-product as a binder on the compressive strength,
microstructure, and swelling potential of the mixed soil, which has hardly been studied. Moreover,
in this work, the deformability of the soil with the additive has been studied. The soil is going to be
used as an embankment in a real project, where the water table level is near the ground surface, so the
natural water content of the soil is high. The dry mixing method for soil mixing using cement as the
binder, where the cement is added directly to the sample, is more efficient when the moisture content
of the natural soil is high [32], and it is the common procedure when soft soils are encountered near
the surface. Therefore, in this study, the limestone powder is added dry to the soil with the natural
water content. Finally, deformability and strength properties of the mixed soil are studied by physical
and mechanical tests.

2. Materials and Methods

2.1. Materials

2.1.1. Soil
The soil used in this study was a natural clayey soil from the Almeria province, southern Spain.
Table 1 shows the main geotechnical properties of this soil. It is classified as a medium-low plasticity
clay (CL) according to the Unified Soil Classification System (USCS) [33]. The mineralogical and
chemical characterization of the soil was performed by means of X-Ray Diffraction (XRD) and X-Ray
Fluorescence (XRF), respectively. The results obtained in these tests are shown in Figure 2 and Table 1.

Table 1. Main geotechnical properties of the soil used in this study.

Property Value Property Value

% Sand (0.06–2 mm) 15 Plasticity Index 20.8
% Silt (0.002–0.06) 60 Activity 0.83
% Clay (<0.002 mm) 25 Free swelling 5.70 1
Liquid Limit 44.6 Particle density (kN/m3 ) 26.0
Plastic Limit 23.8 Soil classification (USCS) CL
1 For a natural water content of 12%.

The semiquantitative mineralogical analysis performed using XRD shows that tested soil sample
consists of illite 28.7%, calcite 22.5%, quartz 19.4%, gypsum 7.6%, montmorillonite 5.9%, and kaolinite
3.9%. According to this analysis, the predominant clay mineral in the soil is illite, which is consistent
with the activity of the soil shown in Table 1. Normal clays usually present an activity between 0.75 to
1.25, with 0.90 being a common value for illite minerals [34]. A medium to high swelling potential,
such as that obtained in the free swelling test, is expected for a soil with the geotechnical properties,
percentage of clay, and activity shown in Table 1 [35].
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Figure 2.
Figure
Figure 2. XRD
2. XRD results
XRD results for
results for the clayey
for the
the clayey soil.
clayey soil.
soil.

2.1.2. Additive
2.1.2. Additive
The additive
additive used
usedininthis thisresearch
researchwas limestone powder waste, obtained from aa dumpsite
dumpsite of aa
was limestone powder waste, obtained from a dumpsite
The additive used in this research was limestone powder waste, obtained from of
natural
of a stone
natural industry
stone industryfrom cutting
from cuttingand polishing
and polishing works.
works.ThisThis
natural stone industry from cutting and polishing works. This additive is mainly composed of additive is
additive mainly
is mainly composed
composed of
carbonates
of carbonates (CaCO 3 and
(CaCO CaMg(CO
and CaMg(CO 3)2). 3The
)2 ). results of
The results the DRX
of the and
DRXFRX
carbonates (CaCO3 and CaMg(CO3)2). The results of the DRX and FRX analysis are shown in Figure
3 andanalysis are
FRX analysis shown in
are shownFigurein
33 and
and Table
Table
Figure 3 and 2, respectively.
Table The mineral
2, respectively. mineral
The mineral composition
compositionof the
the oflimestone
limestone powder
the limestone obtained
powder by aa
obtained
2, respectively. The composition of powder obtained by
quantitative
by a analysis
quantitative of
analysisthe DRX
of results
the DRX is calcite
results 67.8%
is calciteand dolomite
67.8% and 26.1%. In
dolomite
quantitative analysis of the DRX results is calcite 67.8% and dolomite 26.1%. In this study, the additive this study,
26.1%. Inthe additive
this study,
is expected
the
is expected
additivetoiswork as aa filling
expected
to work as filling
to work material
as a because
material the effects
filling material
because the effects of the
the addition
because
of addition
the effectsareofstudied
are studied only in
the addition
only in the
the
are
short term.
studied
short term. Nevertheless,
only Nevertheless, the
in the short the calcium
term. calcium carbonate
Nevertheless, carbonate composition
the composition of
calcium carbonateof the
the additive
additive could
composition could generate
of the generate
additive
pozzolanic
could reactions
generate between
pozzolanic the calcium
reactions ions
between and thethe silica
calcium and
ionsalumina
pozzolanic reactions between the calcium ions and the silica and alumina of the clay minerals in and of
the the clay
silica minerals
and alumina in the
the
of
long
the term.
clay These
minerals reactions
in the can
long bring
term.the formation
These of
reactionscementitious
can bring products,
the
long term. These reactions can bring the formation of cementitious products, such as calcium-silicate- such
formation as calcium-silicate-
of cementitious
hydrates (C-S-H),
products,
hydrates (C-S-H), calcium-aluminate-hydrates
such as calcium-aluminate-hydrates
calcium-silicate-hydrates (C-S-H), (C-A-H),calcium-aluminate-hydrates
(C-A-H), and calcium-aluminium-silicate-hydrates
and calcium-aluminium-silicate-hydrates
(C-A-H), and
(C-A-S-H) [24].
[24]. Previous
Previous works
works reported
calcium-aluminium-silicate-hydrates
(C-A-S-H) reported the formation
(C-A-S-H)
the formation ofPrevious
[24]. of cementing
cementing and poorly
works
and poorly
reported crystalline gels when
the formation
crystalline gels when of
calcium carbonate
cementing
calcium carbonate with
and with lime
poorly lime was
was added
crystalline added to
gels when to clays
clays [36].
calcium[36].carbonate with lime was added to clays [36].

Figure 3. XRD results for the additive.

Figure 3. XRD results for the additive.
2.1.3. Mixed Soil
2.1.3. Mixed
2.1.3. Mixed Soil
Soil
As this research intends to simulate the real mixing of the soil and the additive in the field,
As this
As this research
research intends to to simulate thethe real mixing
mixing of of the
the soil
soil and
and the
the additive
additive inin the
the field,
field, the
the natural moisture intends
content of simulate
the soil was real
used to prepare the samples. The soil was dried inthean
natural
natural moisture content of the soil was used to prepare the samples. The soil was dried in an oven
oven
oven at moisture
40 ºC to acontent
constant ofweight;
the soilafterwards,
was used tothe prepare
materialthewas
samples. The soil was
disaggregated anddried
passedin through
an
at 40
at 40 ºC toto a constant
constant weight;
weight; afterwards,
afterwards, thethe material waswas disaggregated and and passed
passed through
through aa 0.40
0.40
a 0.40ºCmm asieve. Subsequently, 31% of watermaterial
by total dry disaggregated
weight of the soil was added, obtaining
mm
mm sieve. Subsequently,
sieve. Subsequently, 31%
31% of water
of water by total
by content dry weight
total dryasweight of the
of the soil was
soil was added,
added, obtaining
obtaining aa
a homogeneous soil with the same moisture in the field. Finally, samples were prepared
homogeneous
homogeneous soil
soil with the same moisture content as in the field. Finally, samples were prepared by
by adding 5, 10, 15,with the same
20, and 25% of moisture content dust
dry limestone as in by
thetotal
field.dry
Finally,
weight samples
of the were prepared
soil. The samplesby
adding
adding 5, 10, 15, 20,
5, 10, 15,afterand
20, and 25% of
25% the dry
of dry limestone
limestone dust by total dry weight of the soil. The samples were
were prepared mixing additive and dust
storedbyintotal dry weight
a curing roomof atthe soil. The samples
a controlled were
temperature
prepared ◦after
prepared after mixing
mixing the
the additive
additive and
and stored
stored inin aa curing
curing room
room atat aa controlled
controlled temperature
temperature of of 20
20 ±± 22
of 20 ± 2 C and 95% of relative humidity for 7 days, after which they were tested. Every test was
°C and
°C and 95%
95% of of relative
relative humidity
humidity for for 77 days,
days, after
after which
which they
they were
were tested.
tested. Every
Every test
test was
was performed
performed
Sustainability 2019, 11, 679 5 of 14

performed in triplicate per each dosage, except for the unconfined compressive strength test of the
natural soil, which was performed over five samples.

Table 2. The chemical composition of the soil and the additive determined by FRX analysis.

Compound Soil Mass % Additive Mass %

Na2 O 0.919 0.183
MgO 5.290 5.085
Al2 O3 13.902 0.571
SiO2 36.669 1.353
P2 O5 0.316 0.139
SO3 2.760 0.273
Cl 0.248 0.101
K2 O 2.907 0.105
CaO 14.722 62.658
TiO2 0.644 0.036
Cr2 O3 0.018 0.258
MnO 0.070 0.034
Fe2 O3 5.461 0.041
SrO 0.175 –

2.2. Methods

2.2.1. X-Ray Diffraction

The soil and the additive were characterized by XRD using a Bruker D8-Advance X-Ray
diffractometer (Bruker, Billerica, MA, USA), with a high-temperature Chamber (up to 900◦ C), with a
generator of x-ray KRISTALLOFLEX K 760-80F (Bruker, Billerica, MA, USA, power: 3000W, voltage:
20–60KV and current: 5-80mA) with a tube of RX with a copper anode.

2.2.2. X-Ray Fluorescence

The soil and the additive were characterized by an X-ray sequential spectrometer PHILIPS MAGIX
PRO (Philips, Amsterdam, Netherlands) equipped with a rhodium X-ray tube and beryllium window.
PW2400 spectrometer (Philips, Amsterdam, Netherlands) is a sequential instrument with a single
goniometer based measuring channel, covering the complete measuring range.

2.2.3. Atterberg Limits

The Atterberg limits of the soil were determined using the Spanish standards UNE 103103 [37]
for the Liquid Limit and the UNE 103104 [38] for the Plastic Limit, corresponding both standards to
ASTM D 4318 [39].

2.2.4. Free Swell Index

The tests for the assessment of the free swelling of the soil in the oedometer device were conducted
according to the UNE 103601 [40] and the ASTM D4546 [41]. The samples for the swelling tests were
prepared by adding 12% of water to the dry natural soil to better understand the effect of the additive
on the swelling potential. This water content corresponds to the lowest interval value of the optimum
moisture content for compacting clays according to Carter and Bentley [42], which allows observation
of the swelling potential of the soil. Afterwards, samples were prepared by adding 5, 10, 15, 20 and
25% of dry limestone dust by total dry weight of the soil. All the samples were compacted with an
energy source corresponding to the Standard Proctor compaction energy. Each sample had a diameter
of 50 mm and an initial height of 20 mm. Eighteen free swelling tests were performed—three tests per
each dosage and three for the natural soil.
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2.2.5. Unconfined Compressive Strength

2.2.5.The Unconfined
Unconfined Compressive
Compressive Strength (UCS) of the natural and mixed soil were determined
Strength
according to the standards UNE 103400 [43] and ASTM D2166 [44]. The unconfined compressive
The is
strength Unconfined
equal to theCompressive
maximum value Strength (UCS) of the
of compressive natural
stress and
or the mixed soilstress
compressive were atdetermined
15% axial
according to the standards UNE 103400 [43] and ASTM D2166 [44]. The unconfined
strain, whichever is secured first. All the samples were compacted with an energy corresponding to compressive
strength is equal
the Standard to the
Proctor maximumenergy.
compaction value ofEach
compressive
sample had stress or the compressive
a diameter of 50 mm andstress at 15%height
an initial axial
strain, whichever is secured first. All the samples were compacted with an energy
of 100 mm. The loading rate was 1 mm/minute, being the UCS maximum strength value obtained corresponding to
the Standard Proctor compaction energy. Each sample had a diameter of 50 mm and an initial
from the start of the test up to a deformation equal to 15% of initial vertical height. Three tests per height of
100 mm.and
dosage Thefive
loading ratenatural
for the was 1 mm/minute, being themaking
soil were performed, UCS maximum
a total ofstrength value obtained
20 unconfined from
compressive
the start
tests. of the test up to a deformation equal to 15% of initial vertical height. Three tests per dosage
and five for the natural soil were performed, making a total of 20 unconfined compressive tests.
2.2.6. One-dimensional Consolidation
2.2.6. One-dimensional Consolidation
The 1-D consolidation tests were performed according to the Spanish Standard UNE 103405 [45]
The 1-D consolidation tests were performed according to the Spanish Standard UNE 103405 [45]
for 0, 5, 10, 15, 20, and 25% of limestone waste powder addition. All the samples were compacted
for 0, 5, 10, 15, 20, and 25% of limestone waste powder addition. All the samples were compacted with
with an energy corresponding to the Standard Proctor compaction energy. Tests were conducted
an energy corresponding to the Standard Proctor compaction energy. Tests were conducted under
under the loading path of 5, 10, 20, 50, 100, 200, 400, and 800 kPa and an unloading path of 400, 200,
the loading path of 5, 10, 20, 50, 100, 200, 400, and 800 kPa and an unloading path of 400, 200, 100, 50,
100, 50, and 20 kPa. Each sample had a diameter of 50 mm and an initial height of 20 mm. A total of
and 20 kPa. Each sample had a diameter of 50 mm and an initial height of 20 mm. A total of 18 1-D
18 1-D consolidation tests were performed—3 tests per each dosage and 3 for the natural soil.
consolidation tests were performed—3 tests per each dosage and 3 for the natural soil.
2.2.7. Scanning
2.2.7. Scanning Electron Microscopy (SEM)
Electron Microscopy (SEM)
The structure
The structure of
of the
thenatural
naturalsoil
soiland
andthe
thesoil
soilwith
with20%
20%ofoflimestone
limestonepowder
powderwere
wereexamined
examinedusing
using
a
a JEOL JSM-840 Scanning Electron Microscope (SEMTech Solutions, Billerica, MA,
JEOL JSM-840 Scanning Electron Microscope (SEMTech Solutions, Billerica, MA, USA). The acceleratingUSA). The
accelerating
voltages usedvoltages
for this used
workfor thissetwork
were were10
between setand
between
15 kV. 10Theand 15 kV.were
samples The made
samples were made
conductive by
conductive by coating
coating them with gold. them with gold.

3. Results
3. Results

3.1. Atterberg
3.1. Limits
Atterberg Limits
The results
The results of
of the
the Atterberg
Atterberg limits
limits are
are shown
shown in in Figure
Figure 4.4. As
As can
can be
be seen
seen in this figure,
in this figure, aa clear
clear
decrease is
decrease is observed
observed inin Liquid
Liquid Limit
Limit (LL)
(LL) and
and Plasticity
Plasticity Index
Index (PI)
(PI) when
when limestone
limestone powder
powder isis added.
added.
LL and
LL and PI
PI values
values decrease
decrease from
from 44.6
44.6 and
and 20.8
20.8 to
to 37.2
37.2 and
and 14.1,
14.1, respectively.
respectively. This
This decrease
decrease corresponds
corresponds
to aa reduction
to reduction ofof 17%
17% for
for the
the LL
LL and
and ofof 32%
32% for
for PI
PI when
when the
the additive
additive is
is added.
added. The
The addition
addition ofof this
this
binder seems
binder seems toto have
have little
little influence
influence onon the
the value
value of
of the
the Plastic
Plastic Limit
Limit (PL),
(PL), remaining
remaining approximately
approximately
constant for
constant for the
the natural
natural soil
soil and
and the
the mixed
mixed soil
soil

Figure
Figure 4.
4. Effect
Effect of
of limestone
limestone powder
powder content
content on
on the
the Atterberg limits of
Atterberg limits of stabilized
stabilized clay.
clay.
Sustainability 2018, 10, x FOR PEER REVIEW 7 of 14
Sustainability 2019, 11, 679 7 of 14

3.2. Free swell index

Theswell
3.2. Free results of the percentage of free swell for samples prepared by adding from 0 to 25% of
index
limestone
The results of are
powder the depicted
percentagein Figure
of free 5. Freefor
swell swelling
samples is reduced
preparedfrom 5.70% for
by adding fromnatural soil of
0 to 25% to
3.33% when only 5% of limestone powder is added. For additions higher than 5%, less
limestone powder are depicted in Figure 5. Free swelling is reduced from 5.70% for natural soil to reduction is
achieved,
3.33% when obtaining
only 5%values of 2.39,powder
of limestone 2.22, andis 2.49%
added.ofFor
freeadditions
swellinghigher
for 10,than
15, and
5%,20%
less of limestone
reduction is
powder, respectively. On the contrary, an increase up to 3.90% is observed for mixed soil
achieved, obtaining values of 2.39, 2.22, and 2.49% of free swelling for 10, 15, and 20% of limestone with 25%
dust.
powder, respectively. On the contrary, an increase up to 3.90% is observed for mixed soil with 25% dust.

Figure 5. Effect of limestone powder content on the free swell index of the stabilized clay.
Figure 5. Effect of limestone powder content on the free swell index of the stabilized clay.
3.3. Unconfined Compressive Strength
3.3. Unconfined Compressive Strength
Axial strain versus axial stress relation for all the tested samples is shown in Figure 6a. The natural
Axial strain
soil samples versus
present axial stress
a typical relation
parabolic shapefor with
all the testeddeviation
a small samples isinshown
the five in tested
Figuresamples.
6a. The
natural soil samples present a typical parabolic shape with a small deviation
This stress-strain behavior changes from the parabolic to a bilinear shape when limestone powder in the five tested
is
samples.
added. InThis
thesestress-strain behavior
bilinear curves, changes
the initial slopefrom the parabolic
is similar for all thetosamples,
a bilinear shape when
regardless limestone
of the amount
powder
of is added.
addition. In these the
Nevertheless, bilinear
second curves,
slopethe initial
of the curveslope is similar
increases for amount
as the all the samples, regardless
of limestone powderof
the amount
increases. Allofthe
addition.
samples, Nevertheless,
with and withoutthe second
addition,slope of thea curve
present ductileincreases
behavioraswithout
the amount of
defined
limestone powder increases. All the samples, with and without addition, present
peak stress. Due to this ductile behavior, the UCS is obtained as the axial stress when the axial strain is a ductile behavior
without
equal to defined
15%. peak stress. Due to this ductile behavior, the UCS is obtained as the axial stress when
the axial
The strain
resultsisof
equal to 15%.
the UCS for samples prepared by adding from 0 to 25% limestone powder are
The results of the
depicted in Figure 6b. As canUCS forbesamples
seen in prepared
this figure, bythe
adding from 0 to as
UCS increases 25%thelimestone
amount ofpowder are
limestone
depicted in Figure 6b. As can be seen in this figure, the UCS increases as
powder increases. Nevertheless, the rate of increase is much higher from 0 to 20% of addition than the amount of limestone
powder
from increases.
20 to 25%, whereNevertheless, the rate
the line is nearly of increase
horizontal. The is effect
muchof higher frompowder
limestone 0 to 20% of addition
content on thethan
E50
from 20 to 25%, where the line is nearly horizontal. The effect of limestone
soil modulus and strain at 50% of the maximum stress is also shown in Figure 6b. An upward general powder content on the
E50 soil modulus and strain at 50% of the maximum stress is also shown in Figure 6b. An upward
trend can be seen in the E50 modulus as the limestone dust increases from 0 to 20%. Nevertheless,
general
the trend candecreases
E50 modulus be seen from
in the20E50 modulus
to 25% as the Itlimestone
of addition. dust increases
is worth noting from 0 to
that the upward 20%.
general
Nevertheless, the E50 modulus decreases from 20 to 25% of addition. It is worth noting that the
trend from 0 to 25% is more evident if the outlier, which presents a high value of E50 for 5% of addition,
upward general trend from 0 to 25% is more evident if the outlier, which presents a high value of E50
is deleted.
for 5% of addition, is deleted.
Sustainability 2019, 11, 679 8 of 14
Sustainability 2018, 10, x FOR PEER REVIEW 8 of 14

(a) (b)
Figure
Figure 6. 6.Effect
Effectofoflimestone
limestonepowder
powder content
content onon the
the Unconfined
Unconfined Compressive
CompressiveStrength
Strength(UCS) of of
(UCS)
stabilized
stabilized clay.
clay. (a)(a) Axial
Axial strainvs.
strain vs.axial
axialstress;
stress;(b)
(b) limestone
limestone powder
powdercontent
contentvs.
vs.UCS
UCSand
andE50E.50 .

3.4.3.4. One-dimensionalconsolidation
One-dimensional consolidation
The
The normalizedvoid
normalized voidratio
ratioversus
versuslog
logstress
stress relationship
relationship forforthe
thethree
threesamples
samplesofofnatural
naturalsoil and
soil and
thethe mixed
mixed soil
soil is isshown
shownininFigure
Figure7.7. As
As can
can be
be seen
seen inin this
this figure,
figure,aageneral
generaltrend
trendofofreducing
reducing thethe
normalized
normalized voidratio
void ratiofor
forthe
thelast
laststeps
steps of
of the
the loading
loading path
path (800
(800kPa)
kPa)isisobserved
observedasasthetheamount
amount of of
limestone powder increases. Two 1-D consolidation curves, one for the natural
limestone powder increases. Two 1-D consolidation curves, one for the natural soil and the other for soil and the other for
20%20% additive,
additive, showshow anomalous
anomalous values
values in in
twotwo steps
steps of of
thethe loading
loading path
path (Figure
(Figure 7).7). Therefore,
Therefore, these
these two
two curves were not taken into consideration in the calculation of the Compression
curves were not taken into consideration in the calculation of the Compression (Cc ) and the Swelling (C c) and the

(CsSwelling (CC
) indexes. s) indexes. Cc expresses the relative compressibility of the soil and is determined from the
c expresses the relative compressibility of the soil and is determined from the straight
straight portion of the loading path of the void ratio versus log stress relationship. Cs was obtained
portion of the loading path of the void ratio versus log stress relationship. Cs was obtained from the
from the slope of the unloading straight portion of the same curves. The effect of limestone powder
slope of the unloading straight portion of the same curves. The effect of limestone powder content on
content on the Cc and Cs of the stabilized clay is depicted in Figure 8. The general trend observed in
the Cc and Cs of the stabilized clay is depicted in Figure 8. The general trend observed in Figure 7 is
Figure 7 is more evident in Figure 8, as Cc, and also Cs, decreases from 0 to 25% of additive content.
more evident in Figure 8, as Cc , and also Cs , decreases from 0 to 25% of additive content.
Sustainability 2019, 11, 679 9 of 14
Sustainability 2018, 10, x FOR PEER REVIEW 9 of 14

Figure 7. Normalized
Figure 7. Normalized void
voidratio
ratioversus
versuslog
logstress
stress relationship
relationship forfor
thethe natural
natural soil,soil, 5, 15,
5, 10, 10, 20,
15,and
20, and
25%
25% of limestone powder content.
of limestone powder content.

Figure
Figure 8. 8. Effect of limestone
Effect of limestone powder
powder content
content on
on the
the Compression
Compression index
index (C
(Ccc)) and
and the
the Swelling
Swelling index
index
(C
(Css)) of
of the
the stabilized
stabilized clay.
clay.

3.5.
3.5. Scanning
Scanning Electron
Electron Microscopy
Microscopy

The
The microstructures
microstructures of of the
the natural
natural soil
soil and
and the
the soil
soil with
with 20%
20% of
of limestone
limestone powder
powder areare shown
shown inin
Figure 9a and Figure 9b, respectively. The microtexture of the natural soil is significantly modified
Figures 9a and 9b, respectively. The microtexture of the natural soil is significantly modified by the
by the addition
addition of the limestone
of the limestone powder. powder. The untreated
The untreated naturalnatural soil presents
soil presents a lessacompact
less compact structure
structure than
than that observed in the treated soil. Clean clay particles are observed in the SEM image of soil,
that observed in the treated soil. Clean clay particles are observed in the SEM image of the natural the
natural soil,
whilst the whilst
image the soil
of the image of the
with theadditive
soil withshows
the additive shows these
these particles covered particles
and porecovered
spacesand pore
filled by
spaces filled by fine aggregates.
fine aggregates.
Sustainability 2019, 11, 679 10 of 14
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Figure 9. SEM
Figure 9. SEM images
images of
of (a)
(a) natural
natural soil,
soil, and
and (b)
(b) natural
natural soil
soil with
with 20%
20% of
of limestone
limestone powder
powder addition
addition
after 7 days of curing.
after 7 days of curing.
4. Discussion
4. Discussion
The results obtained show a general positive effect of the addition of limestone powder to
The results obtained show a general positive effect of the addition of limestone powder to clayey
clayey soils.
soils.Although the Atterberg limits of the soil do not show a big change when the waste is added,
Although the Atterberg limits of the soil do not show a big change when the waste is added, the
the Liquid Limit and the Plasticity Index present a clear decrease with the addition of the dust.
Liquid Limit and the Plasticity Index present a clear decrease with the addition of the dust. Similar
Similar results were found by Sabat and Muni [30] when adding limestone dust to an expansive clay,
results were found by Sabat and Muni [30] when adding limestone dust to an expansive clay, for
for Sirvrikaya et al. [23] for marble dust addition, and for Igwe et al. [46] when granite and dolerite
Sirvrikaya et al. [23] for marble dust addition, and for Igwe et al. [46] when granite and dolerite dust
dust was added to a clayey soil. Nevertheless, the reduction obtained in this work was a little higher.
was added to a clayey soil. Nevertheless, the reduction obtained in this work was a little higher.
Regarding the effect of the limestone powder addition on the free swelling of the soil, a general
Regarding the effect of the limestone powder addition on the free swelling of the soil, a general
trend is observed of reduction of the index when this industrial by-product is added. Free swelling
trend is observed of reduction of the index when this industrial by-product is added. Free swelling
is reduced from 5.70% for natural soil to 3.33% when only 5% of limestone powder is added.
is reduced from 5.70% for natural soil to 3.33% when only 5% of limestone powder is added. This
This constitutes a reduction of 42% in the free swelling of the mixed soil. As stated above, smaller
constitutes a reduction of 42% in the free swelling of the mixed soil. As stated above, smaller relative
relative reductions of the free swelling are achieved when the amount of additive is increased.
reductions of the free swelling are achieved when the amount of additive is increased. A reduction
A reduction of 58, 61, and 56% are observed when the limestone powder addition is of 10, 15, and 20%,
of 58, 61, and 56% are observed when the limestone powder addition is of 10, 15, and 20%,
respectively. Only a reduction of 31% is obtained for 25% of limestone powder, breaking the downward
respectively. Only a reduction of 31% is obtained for 25% of limestone powder, breaking the
trend observed from 0 to 20%. A decrease in the swelling index up to the maximum amount of marble
downward trend observed from 0 to 20%. A decrease in the swelling index up to the maximum
dust addition was found by previous research [24,26], although Ali et al. [26] only studied a maximum
amount of marble dust addition was found by previous research [24,26], although Ali et al. [26] only
addition of 12%. Ogila [29] reported a decrease between 30 to 45% of the heave percentage when 20%
studied a maximum addition of 12%. Ogila [29] reported a decrease between 30 to 45% of the heave
of limestone dust was added to three different clayey soils, similar to results obtained by Sabat and
percentage when 20% of limestone dust was added to three different clayey soils, similar to results
Muni [30], although in that case the maximum limestone powder added was 12%. The increase of the
obtained by Sabat and Muni [30], although in that case the maximum limestone powder added was
swelling index for 25% of limestone powder is probably due to the considerable increase of matric
12%. The increase of the swelling index for 25% of limestone powder is probably due to the
suction caused by the reduction of the initial water content of the samples, since the dust is added dry
considerable increase of matric suction caused by the reduction of the initial water content of the
to the wet soil.
samples, since the dust is added dry to the wet soil.
The Unconfined Compressive Strength of the mixed soil increases with the amount of limestone
The Unconfined Compressive Strength of the mixed soil increases with the amount of limestone
powder, obtaining an increase of 31, 60, 98, 142, and 148% when 5, 10, 15, 20, and 25% of waste
powder, obtaining an increase of 31, 60, 98, 142, and 148% when 5, 10, 15, 20, and 25% of waste is
is added, respectively. These results show a clear improvement of the compressive strength of the
added, respectively. These results show a clear improvement of the compressive strength of the soil
soil with the addition of this by-product. According to Ni et al. [47], the contribution of fines to the
with the addition of this by-product. According to Ni et al. [47], the contribution of fines to the
compressive strength of mixed soils depends on the relative hardness between the fines and the coarser
compressive strength of mixed soils depends on the relative hardness between the fines and the
grains. If fines are harder than the coarser grains, their presence can have a positive contribution in
coarser grains. If fines are harder than the coarser grains, their presence can have a positive
the compressive strength of the soil. Although the soil studied in the present research is not a mixed
contribution in the compressive strength of the soil. Although the soil studied in the present research
soil, in addition to the binder effect of the limestone dust, a similar effect to the one described by
is not a mixed soil, in addition to the binder effect of the limestone dust, a similar effect to the one
Ni et al. [47] can occur. As stated in Section 2.1.1, the natural soil consists mainly of illite, calcite,
described by Ni et al. [47] can occur. As stated in subsection 2.1.1, the natural soil consists mainly of
quartz, gypsum, montmorillonite, and kaolinite (Figure 2). All these minerals, except for quartz and
illite, calcite, quartz, gypsum, montmorillonite, and kaolinite (Figure 2). All these minerals, except for
calcite, present a hardness in Mohs scale lower than the fines provided by the additive that fill the
quartz and calcite, present a hardness in Mohs scale lower than the fines provided by the additive
voids (Figure 9), mostly composed of calcite and dolomite (Figure 3). Therefore, the added fines have a
that fill the voids (Figure 9), mostly composed of calcite and dolomite (Figure 3). Therefore, the added
Sustainability 2019, 11, 679 11 of 14

higher hardness than most of the particles presented in the natural soil and could be responsible for
the observed increase of compressive strength of the soil.
The UCS rate of increase is much higher from 0 to 20% of addition than that observed from 20
to 25%. This could mean that there is a threshold in the beneficial effect of the addition at around
20%. Similar results were obtained by Saygili [24] and Sabat et al. [25], although in this last study the
UCS and the California Bearing Ratio (CBR) show a maximum value for 20% of marble dust and a
decrease for 25 and 30% of this addition. Sabat and Muni [30] also found a threshold value when
adding limestone dust to an expansive soil, although in this case it was found for 9% of addition.
The stress-strain behavior when the limestone powder is added shows a progressive change from a
parabolic curve to a bilinear one. This bilinear behavior is more pronounced as the amount of addition
is higher. The slope of the second part of the curve also increases as the amount of limestone powder
increases. This behavior could be due to the addition of a non-cohesive material to the clayey soil.
For this reason, as the amount of limestone waste increases, the mixed soil stress-strain behavior moves
away from the common behavior of soft soils.
The E50 soil modulus also shows an upward general trend from 0 to 20%, being increased by 67,
103, 80, and 115% when 5, 10, 15, and 20% of dust is added, respectively. As said above, this trend
is more evident if the two anomalous values, which present high values of E50 , are deleted, one for
5 and another for 10%. In this case, the increase was 7, 77, 80, and 115%. A reduction of the E50 is
observed from 20 to 25% of limestone dust. According to these results, the soil tends to not only
increase its compressive strength but also its stiffness when limestone powder is added. This is in
line with the general trends found in previous works [48,49], where an increase in the E50 modulus
was observed when the UCS increased. According to Ayeldeen et al. [50], E50 can be estimated for
disturbed cement-stabilized soft clay as between 25 to 50 times UCS. Other authors increase this value
to between 50 to 150 times [51]. Nevertheless, the ratio obtained in the present study is a little smaller,
with E50 = 17 UCS (R2 =0.88) when considering the results from 0 to 20% of addition, and E50 = 16 UCS
(R2 =0.47) when considering the results from 0 to 25%. The anomalous results of E50 have not been
taken into account in either of these values.
Ayeldeen et al. [50] reported that undisturbed cement-stabilized clay, with higher ratios E50 /UCS,
up to 160, shown brittle behavior with a clear peak. Nevertheless, re-molded samples with lower ratios
have shown a ductile strain-stress behavior without a clear peak. Similar behavior has been observed
in the present research. When limestone powder is added to the clayey soil, small ratios E50 /UCS are
reported, with a ductile behavior being observed.
The increase in the stiffness of the soil when limestone powder is added is confirmed by the
decrease of the soil compressibility when it is tested in the oedometer apparatus. The compression
index, which is a direct indication of the tendency of a clayey soil to settle when it is loaded, decreases
as the amount of additive increases. The Cc index is reduced by 3, 13, 5, 20, and 27% when 5, 10, 15,
20, and 25% of dust is added, respectively. A similar trend is observed for Cs index as the amount
of limestone powder increases, with a maximum reduction of 31% when 25% of powder is added.
Therefore, this addition decreases the compressibility of the soil as the slope of the virgin and rebound
consolidation curves are reduced. This lower compressibility of the mixed soil is attributed to the fine
aggregates of the limestone powder dust filling the voids of the natural soil. The SEM images shown
in Figure 9 support this idea, as the treated soil presents a more compact structure than that observed
in the natural soil.

5. Conclusions
The effect of the addition of limestone powder to a clayey soil on Atterberg limits, free swelling
index, unconfined compressive strength, compressibility, and microstructure has been studied.
Experimental results show a moderately beneficial effect on the geotechnical properties of the clayey
soil when limestone powder is added that can be summarized as follows:
Sustainability 2019, 11, 679 12 of 14

• There is a reduction of the Liquid Limit and Plasticity Index up to 17 and 32%, respectively, when
25% of the additive is added.
• The reduction of the free swelling index reaches a maximum value of 61% when 15% of powder
is added.
• The unconfined compressive strength increases up to 148% for the maximum percentage
of addition.
• A reduction of the compressibility of the mixed soil is observed. Cc and Cs indexes decreases up
to 27% and 31%, respectively, when the soil is mixed with 25% of limestone powder.
• SEM images show a more compact microstructure of the soil when the limestone powder is added.

Although the addition of limestone powder to clayey soils achieves a moderate improvement on
the geotechnical properties of clayey soils, the use of this addition has a very positive environmental
effect, both by avoiding the use of traditional binders, which have a strong environmental effect on
its manufacturing process, and by avoiding dumping the waste from the natural stone industry into
landfills. It is noteworthy that the environmental benefits of the use of limestone powder, as of any
other binder, will depend on the distance between the quarries, or the storage, and the work.
In conclusion, this research highlights the potential re-evaluation of limestone powder waste as a
binder material for the improvement of clayey soils, enabling reduction of the negative impacts of this
waste and obtaining economic and environmental benefits from its reuse.

Author Contributions: J.L.P., R.T. and M.C. designed the methodology of the research. J.L.P. and E.G. performed
the experiments. R.T. and M.C. supervised the investigation J.L.P. wrote the paper. R.T., M.C. and A.R. reviewed
and edited the manuscript.
Funding: This research was funded by the University of Alicante under the projects GRE17-11.
Acknowledgments: We would like to thank Dr. David Benavente for interpreting the DRX results. We also would
like to thank the company Romanense de Mármoles, S.L. for providing us with the limestone powder waste used
in this research.
Conflicts of Interest: The authors declare no conflict of interest. The funders had no role in the design of the
study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to
publish the results.

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