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Applied Clay Science 102 (2014) 93103

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Applied Clay Science


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

Research paper

Free swell potential of lime-treated gypseous soil


Abdulrahman Aldaood a,b, Marwen Bouasker a, Muzahim Al-Mukhtar a,
a
b

Centre de Recherche sur la Matire Divise, CRMD and Laboratoire PRISME, Universit d'Orlans, France
Mosul University, College of Engineering, Civil Engineering Department, Al-Majmooah Street, Mosul, Iraq

a r t i c l e

i n f o

Article history:
Received 17 March 2014
Received in revised form 4 October 2014
Accepted 24 October 2014
Available online 13 November 2014
Keywords:
Gypseous soils
Lime treatment
Swell potential
Wettingdrying
Curing conditions
Microstructural changes

a b s t r a c t
Lime treatment generally enhances the geotechnical properties of the soils. However, some studies have
reported an adverse effect, especially in the presence of gypsum. To develop an understanding of the underlying mechanisms, a study of ne-grained soil with different amounts of gypsum was carried out. The
inuence of curing conditions (curing period and curing temperature) and wetting-drying cycles on the
swell potential of ne-grained soil with (0, 5, 15 and 25%) gypsum was investigated to assess the longterm behavior of this type of soil (i.e. gypseous soil) when used in the construction of road and pavement
structures. Mineralogical and microstructural studies (porosimetry, X-ray diffraction and scanning electron microscopy) were carried out to evaluate the cementitious materials and the presence of ettringite.
The results show that increasing the gypsum content decreased the swell potential of the untreated soil
samples. On the other hand, the swell potential values of soil samples started decreasing after the rst
wettingdrying cycle then reached equilibrium. Lime treatment results show that the suppression of
swelling in lime-treated soil samples without gypsum was partly lost after the rst cycle, especially for
short curing periods and for both temperature values (20 C and 40 C), while long-term curing periods
(more than 28 days) gave good results with respect to the suppression of swell potential values. Lime
treatment of gypsum-containing samples showed an adverse effect on swell potential. The swell potential
values increased with curing period and curing temperature, due to the formation of ettringite. Lastly,
wettingdrying cycles caused an increase in the swell potential values of gypsum-containing samples,
cancelling out the benecial effect of lime treatment to control swell.
2014 Elsevier B.V. All rights reserved.

1. Introduction
Gypseous soils are the most common type of soils, and exhibit a
variety of engineering properties and behaviors, such as excessive
settlement (collapsing) and low shear strength, especially upon
wetting. This behavior is mainly due to gypsum dissolution induced
by water ow, thus increasing the porosity and permeability of the
soil. Therefore, the construction of engineering structures founded on
gypseous soils is highly risky as they can suffer from several engineering
problems such as cracks, tilting or differential settlement and structure
collapse (Aibn et al., 1998; Cooper, 1998, 2008).
In order to improve the engineering behavior of these soils,
several techniques are available in geotechnical engineering practice such as mechanical stabilization, chemical stabilization, or a
combination of these two methods, to create an improved soil
material that possesses the desired engineering properties (Little,
1995; Puppala et al., 2004). Chemical soil stabilization by lime
(CaO or Ca(OH)2) is a proven technique for improving the strength
of gypseous soils (Kota et al., 1996; Puppala et al., 2003; Yong and
Corresponding author.
E-mail address: muzahim.al-mukhtar@univ-orleans.fr (M. Al-Mukhtar).

http://dx.doi.org/10.1016/j.clay.2014.10.015
0169-1317/ 2014 Elsevier B.V. All rights reserved.

Ouhadi, 2007). The immediate effect of lime stabilization is a


strong exothermic reaction between CaO and water present in the
soil, forming calcium hydroxide. The main chemical reactions that
occur during lime stabilization can be summarized as follows:
CaO + H2O Ca(OH)2

Ca(OH)2 Ca++ +2(OH)

Ca++ +2[OH] + SiO2 CSH silica gel

Ca++ +2[OH] + Al2O3 CAH alumina gel


Cation exchange begins to take place between the ions associated
with the clay particles and the calcium ions of the lime (Bergaya and
Lagaly, 2006; Bergaya et al., 2006). This process is primarily responsible
for modications in the soil engineering properties, such as workability
and reduced plasticity (Al-Mukhtar et al., 2012; Bell, 1996; Little, 1995;

94

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

Mathew and Rao, 1997). In addition to the immediate effect caused by


cation exchange, there is a long-term effect of lime stabilization called
the pozzolanic reaction which produces calcium silicate hydrates
(CSH), calcium aluminate hydrates (CAH), and calcium aluminosilicate hydrates (CASH). Pozzolanic reactions are time and curing temperature dependent and thus the strength develops gradually over a
long period (Al-Mukhtar et al., 2010a,b; Little, 1995).
Environmental conditions such as wettingdrying cycles cause variation in the moisture content of soil, resulting in cyclic swelling and
shrinkage. Soil in nature undergoes volume change in several ways:
swelling or collapsing due to an increase in water content, rebound
due to release of load, settlement due to load application and shrinkage
due to water loss. Another pattern of volume change is soil heave or soil
swell due to the presence of certain chemical elements within the soil
matrix which in the right conditions create crystalline structures and
force the matrix apart as the crystals grow. Generally, when soils
containing soluble sulfates (such as gypsum) are mixed with lime or
other calcium-based stabilizers and given access to water, highly expansive calciumaluminatesulfatehydrate minerals form (Hunter, 1988;
Ouhadi and Yong, 2008; Petry and Little, 1992). In the present state of
knowledge, not all these complex reactions have been completely
identied. The most common and the most inuential mineral for
engineering practice is ettringite.
The crystallization of ettringite is expansive and, in addition, is subjected to further large volume changes as it takes in water. Ettringite formation causes soil heave and cracking of pavement structures, and
these problems lead to a reduction in stability and loss of bearing capacity (Hunter, 1988; Little et al., 2010; Mitchell and Dermatas, 1992;
Puppala et al., 2005). Several studies on gypseous soils have shown
that the onset of problems associated with these soils depends on the
initial sulphate levels in soils prior to chemical stabilization (Adams
et al., 2008; Hunter, 1988; Petry and Little, 1992).
The objective of this study was to identify the impact of wetting
drying cycles on the swell potential of lime-treated gypseous soil. An
attempt has also been made to assess the coupled effects of gypsum
content and curing temperature on the swelling behavior of treated
soil samples at both short and long-term curing periods of up to
360 days. Two curing temperatures were used (20 C and 40 C). The
formation and development of ettringite minerals during curing conditions were monitored. Gypseous soils are found in several countries
across the world, and are present in the majority of arid and semi-arid
zones (FAO, 1990, 1993) The gypsum content varies widely from low,
less than 5%, to very high, sometimes exceeding 50% (Boyadgiev and
Verheye, 1996). In order to conduct a precise parametric study, all the
tested samples were prepared in the laboratory, as literature data
show that the gypsum content in nature varies widely. Thus, to control
the exact percentage of gypsum in the different samples tested and in
order to study a broad range of gypsum soil behavior, samples were
prepared with three percentages of gypsum: 5, 15 and 25% by dry
mass of soil.

2. Materials and methods of testing


2.1. Materials
The soil tested was a ne-grained soil from Jossigny to the east of
Paris, France. The liquid limit (L.L.) was 29%, with a plasticity index
(P.I.) of 8% and the specic gravity of the solid (Gs) was 2.66. Based on
the Casagrande plasticity chart and according to the Unied Soil Classication System (USCS), the soil was classied as a low plasticity clay
soil. The grain size distribution analysis is 17% sand, 64% silt and 19%
clay.
The quicklime added, supplied by the French company LHOIST, is a
very ne lime and passes through an 80 m sieve opening. The activity
of the lime used was 94%.

The gypsum used in this study, supplied by the Merck KGaA company,
Germany, is a very ne gypsum and passes through an 80 m sieve
opening, and with a purity of more than 99%.
2.2. Sample preparation
A standard Proctor compaction effort (ASTM D-698) was adopted in
the preparation of the soil samples. To prepare the soil samples, the
oven-dried soil (2 days at 60 C) was rst crushed and passed through
a 4 mm sieve. After grinding, the required amount of soil was mixed
with gypsum under dry conditions. Then the required amount of water
corresponding to the optimum moisture content of natural soil (11%)
was added to the soilgypsum mixtures. All mixing was done manually,
and proper care was taken to prepare homogeneous mixtures. The mixture was then placed in plastic bags for a mellowing time of 24 h.
For lime treatment, the soil samples were stabilized by 3% lime,
which represents the optimum lime content based on the ASTM
D6276 (2006) which used pH to estimate the soillime proportion requirement for Soil Stabilization. This test is derived from the Eades
and Grim test (1966). The soillime mixtures were rst prepared by
thoroughly mixing dry predetermined quantities of soil, gypsum and
lime to obtain a uniform color. Then the required amount of water
was added and again mixed to obtain a uniform moisture distribution.
The mixture was then placed in plastic bags and left for a 1 h mellowing
time (Little, 1995).
After that, the soil samples were statically compacted in rigid stainless steel rings (71 mm in diameter and 20 mm in height), at a strain
rate of 1 mm/min, until they reached the maximum dry unit weight of
the natural soil (17.7 kN/m3). After compaction, the soil samples (i.e.
soil and the ring) were immediately placed in plastic bags to avoid signicant variations in moisture content till testing. The lime-treated soil
samples were immediately wrapped in cling lm and coated with parafn wax to avoid moisture loss, then left to cure for 2, 7, 28, 180 and
360 days at two temperature values (20 C and 40 C).
2.3. Mineralogical and microstructural analysis
The mineralogical and microstructural aspect of the lime-treated soil
samples was studied using scanning electron microscope (SEM), X-Ray
diffraction (XRD) and mercury porosimetry tests. The main objective of
the mineralogical and microstructural investigations was to determine
changes due to lime treatment and to detect the formation of cementitious materials. These tests were conducted on all the soil samples.
For the scanning electron microscopy test (SEM), the preparation of
the specimens followed the method suggested by Tessier (1984) and
described by Al-Mukhtar et al. (1996) in order to preserve the soil fabric.
Soil samples (volume of 1 cm3) were injected by epoxy x resin,
polished, gold-coated and then scanned by a high resolution scanning
electron microscope (PHILIPS XL 40 ESEM). All the soil samples were
prepared in the same manner.
For XRD observations, fractured samples produced after the unconned compression test were powdered, sieved through a 400 m sieve
and dried for 24 h at 40 C. A PHILIPS PW3020 diffractometer was
used for XRD analysis. The diffraction patterns were determined using
Cu-K radiation with a Bragg angle (2) range between 460 running
at a speed of 0.025/6 s.
Pore size distribution tests were carried out using a Pore Seizer
Porosimeter, in which the mercury pressure was raised continuously
to reach more than 210 MPa and measure the apparent pore diameter
in the range of 3.6 nm to 350 m. The method assumes a cylindrical
pore geometry using a modied YoungLaplace equation, generally referred to as the Washburn equation (Giesche, 2006).

P

1
1

r1 r2

2 cos
rpore

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

It relates the pressure difference across the curved mercury interface


(r1 and r2 describe the curvature of that interface) to the corresponding
pore size (rpore) using the surface tension of mercury () and the contact angle () between the solid and mercury. Pore size distribution data
generated by mercury porosimetry are primarily useful in comparative
studies of similar materials.
The applied mercury pressure and the intruded volume of mercury
were monitored during the test. Before applying mercury tests, soil
samples were dried by lyophilization using an ALPHA 12 Ld Plus
GmbH apparatus to avoid the formation of micro-cracks.
2.4. One-dimensional free swell test
To evaluate the free swell potential of the untreated and limetreated soil samples, a free swell test was performed using the standard
one-dimensional oedometer device, in accordance with the ASTM
standard (D-4546).
At the end of each curing period, the compacted soil samples in the
oedometer rings were placed in a consolidation cell between two
dried porous stones, and a sensitive dial gauge was xed on top of the
consolidation cell to measure the vertical soil displacement (Fig. 1).
After calibration with an initial vertical pressure of 2.75 kN/m2
(representing the weight of the loading plate which is part of the consolidation cell), an initial reading was taken to estimate the swell potential, following which the soil samples were soaked with tap water and
allowed to swell under the vertical pressure (2.75 kPa) at a constant laboratory temperature (25 C 2 C). Timeswell readings were continuously noted during the process. The nal reading of the dial gauge
(which represents the highest reading) was used to calculate the free
swell potential together with the initial height of the soil samples,
using the equation below:
Swell potential

H
 100
Hi

where H is the vertical displacement in mm, which represents the difference between initial and nal readings of the dial gauge, and Hi is the
initial height of the soil sample in mm. The precision of the displacement measurement was 0.001 mm and so the precision of the axial
strain was 0.005%, thus satisfying the ASTM D6026 recommendation
for geotechnical data.
The time required to reach the nal reading of the dial gauge (the
maximum value of vertical displacement) depends on the gypsum content, curing period and curing temperature. Thus, the swell test was
continued to (2448 h) until the dial gauge reading had stabilized.

95

2.5. Cyclic one-dimensional free swell test


This test was performed to investigate the evolution of the free swell
potential of lime-treated soil samples, subjected to wettingdrying cycles, due to ettringite formation. All soil samples were subjected to alternate wettingdrying cycles in the oedometer device. After calibration
with an initial pressure of (2.75 kPa) and recording of the initial reading
to estimate the swell potential, as mentioned in Section 2.4, the soil
samples were soaked with tap water and allowed to swell fully over
24 h. After that, the nal reading was recorded, then the water was
drained from the oedometer cell and the sample kept in the cell for at
least 30 min at room temperature (25 C 2 C), to keep it safe from
any damage.
The wetted sample was then extruded from the cell and oven dried
for 24 h at 60 C. After drying and before starting the next cycle, the soil
sample was cooled at room temperature (25 C 2 C) for 30 min. The
soil samples in the consolidation ring were again placed in the
oedometer cell, xed in the oedometer device and wetted by allowing
them to swell over 24 h. In this test, the untreated and lime-treated
soil samples were subjected to four cycles of alternate wetting and
drying.
3. Results and discussion
3.1. Mineralogical and microstructural changes
Changes in the engineering properties of soils resulting from lime
and gypsum addition can be attributed on the one hand to gypsum dissolution due to water absorption which increases the porosity and the
permeability, and on the other hand to mineralogical changes. XRD
was used to highlight the mineral composition of the natural (untreated) soil and the mineralogical changes induced by the chemical reactions between soil matrixes, as presented in Figs. 2 and 3. As shown,
the main natural (untreated) soil components were kaolinite and illite
as clay minerals, and contained quartz, calcite and feldspars. Once treated by lime and for all gypsum percentages, several new peaks appeared,
indicating the formation of new compounds.
Two observations can be made from the XRD patterns. The rst is
that the intensities of all the kaolinite reections decreased during curing, whatever the gypsum content. This behavior is attributed to the fact
that kaolinite is exhausted by the pozzolanic reaction and is consistent
with the pozzolanic behavior of kaolinite. The second one is that the illite is less involved in the pozzolanic reaction than kaolinite. It is worth
noting that the peaks of quartz mineral did not show a clear reduction

D
Diall gaauge
Water
Rinng suppporrtinng
mlppe
thhe sam

Loa
L adinng pplaate
( plieed prresssuree
(App

2.75
2 5 kP
Pa)

S
Soil saampple
Porrou
us stonne

Fig. 1. Experimental setup for free swelling tests.

0% gypsum

I 002

CAH

15% gypsum

5% gypsum

0% gypsum

Natural soil

0
30

40

50

60

10

20

30

15% gypsum

CSH

5% gypsum

10

20

30

40

50

I003 + Q101

60

15% gypsum
I004

5% gypsum

I 001

I 002

10

20

30

40

50

60

2 ()
Fig. 2. XRD patterns of soil samples cured at 20 C.

during curing and lime treatment, indicating that the quartz was not
substantially attacked by lime.
During curing conditions (curing period and curing temperature),
gypsum addition inuenced the creation (formation) of new reections
such as Ca-hydrates in the samples. With curing, these reections seem
to be reinforced, which means crystallization of these new Ca-hydrates.
As mentioned by Al-Mukhtar et al. (2010a,b, 2012), newly formed Cahydrate cannot be observed by XRD because the phases that form during long-term curing periods (i.e. 180 and 360 days) probably do not
have a well-organized crystalline structure, and therefore X-ray reections are greatly weakened. Second, it is possible that reections from
these phases overlap with both those of primary minerals of natural
soil and/or with the reections formed during 28 days.
To summarize, the major cementitious compounds were calcium silicate hydrates (CSH), calcium aluminate hydrates (CAH) and ettringite

600

400

Natural soil

40

50

60

360 days

25% gypsum
C

L
L

15% gypsum

5% gypsum

0% gypsum

200

Natural soil

I 001

0% gypsum

30

Intensity ( counts/s )

CAH

200
Q

20

CSH

400

10

25% gypsum

600

800

360 days

CAH

2 ()

CSH

CSH + G

G
G

0% gypsum

2 ()
800

I003 + Q101

CAH

5% gypsum

200

Natural soil

15% gypsum

I004

CAH

CSH

I 002

I 001

400

I 001

0% gypsum

200

25% gypsum

600

I004

400

60

180 days

CAH

CSH

I004

CSH + G

CAH

600

50

CAH

25% gypsum

CSH + G

G
G

CAH

180 days

I 002

800

Intensity ( counts/s )

40

2 ()

I 002

CSH + G

800

I003 + Q101

2 ()

CSH

20

CSH

10

I003 + Q101

Intensity ( counts/s )

200

Natural soil

Intensity ( counts/s )

CSH
CAH

400

I 001

200

I004

CSH

5% gypsum

28 days

CSH

15% gypsum
I004

25% gypsum

600

I 002

CAH

CSH + G

25% gypsum

600

400

28 days

Intensity ( counts/s )

I 001

Intensity ( counts/s )

800
G

CAH

CSH + G

800

I003 + Q101

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103


I003 + Q101

96

Natural soil

0
0

10

20

30

40

50

60

2 ()
Fig. 3. XRD patterns of soil samples cured at 40 C.

mineral, which were found in all the gypseous soil samples. Ettringite
is a calcium aluminum sulfate hydrate (Ca6Al2(SO4)3(OH)12 26H2O.)
type mineral which is responsible for the early strength gain and is
known for its potential to cause swell.
In samples cured at 20 C, ettringite crystals were not observed in
SEM images for any of the gypsum percentages used. The ettringite
crystals start to appear at 180 days of curing and for 25% of gypsum.
The average length of these crystals does not exceed 5 m.
In samples cured at 40 C, the ndings are almost the same as at
20 C but an early appearance of ettringite crystals at 28 days for 25%
of gypsum can be observed. Moreover, ettringite crystals seem to be
larger than those observed at 28 and 180 days when the curing temperature was 20 C. This increase in the dimension of ettringite crystals can
be explained by the effect of thermal activation as temperature increased from 20 C to 40 C (Al-Mukhtar et al., 2010b). After 360 days,

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

for all samples cured at 20 C and 40 C, SEM images show a signicant


growth of ettringite crystals (average length of 20 m) and the soil texture seems to be dense. Table 1 illustrates the changes induced in the
fabric of the soil and measured by mercury porosimetry tests. Four
ranges of pores were identied to examine in depth the results of mercury porosimetry and to analyse the effect of gypsum content and curing conditions (temperature and time) on the pore size distribution. In
general, signicant differences in pore size distribution curves were exhibited by the soil samples cured for short periods at a low curing temperature, while there was a slight difference in these curves for samples
cured for longer periods at a high curing temperature; most of these differences were in pores larger than (0.1 and 10 m). The pore size distribution of soil samples after 28 days of curing was consistently coarser
than that after 180 and 360 days of curing. This behavior is attributed
to the fact that the hydration reaction (between lime and gypsum) is
much faster than the pozzolanic reaction. The dissociation of lime produced by the hydration reaction quickly leads to occulation of the
clay particles, which increases the porosity of the clay matrix, whereas
the pozzolanic reaction leads to deposition of CSH and CAH on and
around the occulated clay aggregates, resulting in a reduction in the
pore size of soil samples. The percentage of very small pores less than
or equal to (0.1 m) seems to be unchanged with curing period for
both curing temperatures; it represents about one third of total pores
in the tested samples. The small pores (0.11 m) showed an insignicant reduction with increasing curing temperature from 20 C to 40 C.
The percentage of these pores increases with gypsum content. The
medium-sized pores (110 m) behave inversely to small pores with
curing conditions. Finally, larger pores with more than 10 m pore entrance sizes do not change and remain scarce (about 3%) in all tested
samples. These changes in pore size distribution reveal a global renement of the internal microstructure and the evolution of this soil fabric
induced by the pozzolanic products (CSH and CAH) shown in Figs. 2 and
3. The formation of ettringite, as shown in Figs. 4 and 5 respectively not
only enhanced the inter-cluster bonding strength but also lled the pore
space. Further, the effect of cation exchange and attraction caused clay
particles to move close to each other. These changes in pore size distribution inuence the swell potential.
Gypsum addition affected the pore size distribution of soil samples
by increasing the percentages of small pores, which increased with
high gypsum content (25%) and low curing temperature (20C),
while the large pores did not seem to be signicantly affected by this
addition.
The porosity measured during these tests changes with the amount
of gypsum and the curing temperature in the tested samples: overall, as
the gypsum content increased, porosities formed early during 28 days of
curing increased and as the curing temperature increased from 20 C to
40 C. Moreover, for a xed curing temperature (20 C or 40 C), porosities formed early during 28 days of curing seem to be unchanged with
additional curing time.

97

3.2. Free swell potential


Swell potentials of untreated and lime-treated soil samples
compacted at optimum moisture content (OMC) and maximum dry
unit weight (max) were measured. Fig. 6 shows the swell potential variation of untreated soil samples for different gypsum contents. The swell
potential decreased with increasing gypsum content. This behavior is
attributed to the addition of non-expansive materials (gypsum) and to
a reduction in the soil matrix, especially clay content (due to the complementary substitution method used in sample preparation). The
porosity also decreased with gypsum content, as presented in Table 1,
since gypsum acts mainly as an inert ller and tends to reduce the
swell of the soil samples. The swell potential decrement was larger
when the addition of gypsum increased, and the reduction in swell
potential reached 70% for samples with 25% gypsum. Similar observations were reported by (Yilmaz and Civelekoglu, 2009) during their
study on the effect of gypsum addition on the behavior of expansive
soil (bentonite soil).
For lime-treated soil samples, Fig. 7 shows the effects of curing conditions (temperature and curing period) and gypsum content on the
swell potential. The swell potential of lime-treated soil samples without
gypsum decreased with increasing curing periods and a greater reduction was observed for samples cured at 40 C as compared with samples
cured at 20 C. The swell potential was suppressed at 7 days for soil
samples cured at 40 C and at 28 days for samples cured at 20 C. This
reduction is attributed to lime addition which is known to be an
effective stabilizer that reduces the swell potential of clay soils. For the
gypseous soil samples, after the short curing period (i.e. 2 days) and
for both temperature values, swell potential decreased with gypsum addition. This behavior is due to the presence of unreacted lime and gypsum particles which act as ller materials and tend to reduce the swell
potential, as presented above. After 2 days of curing the swell potential
of soil samples increased with gypsum content up to 5% then decreased
and more swelling occurred for soil samples cured for 28 days. In the
case of lime-treated soil samples containing 5% gypsum, the increase
in swell potential can be explained by the chemical reactions caused
by the presence of gypsum, alumina and lime. These reactions lead to
forming an ettringite nucleus which has the ability to grow when the
requisite chemical compounds become available. According to Wild
et al. (1993), a colloidal product which is a precursor to the formation
of crystalline ettringite initially forms on clay particle surfaces during
moist curing in lime-treated sulfated clay soil. On soaking, this product
imbibes water and swells. The amount of this product that can form is
controlled by the relative amounts of free lime, gypsum and alumina
available. Ettringite is a hydrous calcium alumino-sulfate mineral that
precipitates in environments with high pH values and sufcient sulfate
concentration (Little et al., 2010; Puppala et al., 2005). It forms in the
early stages of hydration of calcium aluminate and has a large swell potential, up to 250% (Adams et al., 2008).

Table 1
Pore size distribution from mercury porosimetry results and porosities of samples.
Results concerned the two curing temperature 2040 C
Gypsum content %

Curing period
day

Very small pores


b0.1 m %

Small pores
0.11 m %

Medium pores
110 m %

Large pores
N10 m %

Porosity by mercury
test %

Initial total
porosity %

28
180
360
28
180
360
28
180
360
28
180
360

2430
3736
4335
3732
4029
3429
3235
4236
3536
3231
3427
3432

4121
3416
3317
3624
3128
3927
4621
3820
5118
5117
4820
5019

3346
2647
2145
2339
2640
2542
1642
1642
1144
1348
1450
1155

33
32
22
34
33
22
53
32
42
43
43
42

26.729.3
27.028.7
25.728.0
26.630.6
30.030.5
27.927.2
28.928.5
28.829.1
29.229.0
29.630.8
30.530.3
30.130.2

33.3

15

25

31.5

30.5

28.6

98

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

28 days

10 m

5%G

10 m

15%G

10 m

25%G

180 days
Ettrin ite
Ettringite

10 m

5%G

10 m

15%G

10 m

25%G

360 days

Ettringite cristals

Ettringite cristals

10 m

5%G

10 m

Ettringite cristals
15%G

10 m

25%G

Fig. 4. SEM images show cementitious materials and ettringite development for soil samples cured at 20 C.

28 days

Ettringite

10 m

5%G

10 m

15%G

10 m

5%G

10 m

15%G

10 m

25%G

180 days

10 m

Ettringite
25%G

360 days

Ettringite cristals

10 m

Ettringite cristals

Ettringite cristals
5%G

10 m

15%G

10 m

Fig. 5. SEM images show cementitious materials and ettringite development for soil samples cured at 40 C.

25%G

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

Free Swell (%)

0
0

10

20

30

Gypsum Content (%)


Fig. 6. Free swell of untreated soil samples with different gypsum content.

Although no crystalline ettringite was observed in soil samples with


5% gypsum, the presence of an amorphous ettringite product which
causes swell can be suggested, as mentioned by (Wild et al., 1999). At
higher gypsum content (more than 5%), the soil samples exhibited
less swelling as compared with samples having 5% gypsum, even if
there were ettringite crystals. This is due to unreacted gypsum particles
which act as inert ller materials, restricting the swell. These samples
also appeared to contribute less to ettringite formation than pozzolanic
reactions and hence small swell potentials were observed at increased
gypsum content. Increasing the temperature from 20 C to 40 C led to
a greater reduction in swell potential. This may be attributed to the thermal activation effect: more cementing materials were formed during

2 days

Free Swell (%)

7 days

28 days
180 days

360 days

2
1
0
0

10

20

30

2 days
7 days
28 days
180 days
360 days

3.3. Cyclic free swell potential

Free Swell (%)

Free Swell (%)

curing at 40 C than during curing at 20 C. In addition, soil samples


cured at 20 C show a higher proportion of macro pores, a coarser
pore structure and high porosity values compared with the soil samples
cured at 40 C. Thus, small pores and porosity give little freedom, if any,
for the clay particles to expand because of the cementitious materials
formed during the curing process. Moreover, a smaller pore size and porosity decreases the soil's ability to retain further water upon wetting
and this in turn reduces the swell potential.
During long-term periods of curing (180 and 360 days), the swell
potential values of soil samples increased with increasing gypsum content, and the maximum values were recorded for the samples cured at
40 C rather than 20 C. For the samples with 25% gypsum and cured
at 20 C, the free swell potential values were 2.1% and 3.5% after 180
and 360 days, respectively, against 2.8% and 4% when the soil samples
were cured for the same periods but at 40 C. When the gypsum content
exceeded 5%, the reaction between soil, lime and gypsum dominated
the limesoil reactions. High swell potential values were recorded at
high gypsum contents. The presence of lime and reactive alumina at
these amounts of gypsum appeared to contribute more to ettringite formation than pozzolanic reactions and hence high swell potential values
were recorded. This observation along with the previous one for the
short-term periods leads to the important conclusion that critical
amounts of calcium, reactive alumina and gypsum must be present in
lime-treated soil to form ettringite.
Ettringite crystal formation and growth are one of the main phenomena of the swell potential of lime-treated gypseous soil. The ettringite
crystals are generally formed in the soil voids during the initial reactions.
This formation is expected to occur within a few days to several weeks
(Kota et al., 1996). These crystals will then start to accumulate with the
combined reactions between soil, lime and gypsum system, at high pH
conditions (more than 10.5). When the existing pore void space of soil
samples cannot accommodate any more ettringite crystals, the soil samples will start to swell. Additional swell potential can be attributed to the
hydration reactions of ettringite minerals formed inside the soil matrix
(Puppala et al., 2005). Another factor that may increase the swell potential with curing period and gypsum content is osmotic swelling. It is suggested in (Mehta, 1983; Wild et al., 1993) that osmotic swelling may take
place within colloidal layers in regions of high sulfate concentration in
close proximity to the developing ettringite rods at the clay particle surfaces. When in a saturated condition, ettringite grows and develops from
this colloidal product. During this growth, colloidal ettringite possesses
the capability of imbibing large amounts of water, dramatically increasing the swelling potential of lime-treated gypseous soil samples.

Soil in nature is often under conditions of changeable water content


and undergoes cyclic wettingdrying. This phenomenon has a marked

Gypsum Content (%)


5

99

2
1

0% G
5% G
15% G
25% G

0
0

10

20

30

Gypsum Content (%)


Fig. 7. Free swell of lime treated soil samples with curing periods (A) at 20 C and (B) at
40 C.

0
0

2
3
No. of Cycle

Fig. 8. Cyclic free swell of untreated soil samples with wettingdrying cycles.

100

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

inuence on the properties of soil. Fig. 8 shows the swell potential of untreated soil samples with different amounts of gypsum, corresponding
to the number of wettingdrying cycles. The swell potential of untreated soil samples decreased with increasing wettingdrying cycles. The
maximum signicant reduction in the swell potential values was recorded after the rst cycle and this reduction gradually reached equilibrium at the 4th wettingdrying cycle. Further, it is observed that the
effects of wettingdrying cycles on the swell potential of the untreated
soil samples depended on the amount of gypsum addition: the maximum reduction in swell potential occurred for samples with a high gypsum content (i.e. 15% and 25%). At the same time, it was observed that
the trend of reduction in swell potential of soil samples without gypsum
is similar to that of samples with gypsum. The reduction in swell potential is attributed to destruction of the soil matrix (especially the clay
structure matrix) during wettingdrying cycles, as well as to partial
breakdown of the soil particles by reconstruction of the structure of aggregates that occurred during these cycles (Yazdandoust and Yasrobi,
2010). The results obtained in this investigation are in agreement with
those reported by (Dif and Bluemel, 1991; Guney et al., 2007). During
wettingdrying cycles, the soil samples without gypsum cracked as a result of shrinkage and low tensile strength, whereas there were no obvious cracks in the gypseous soil samples, especially those with higher
gypsum content, as shown in Fig. 9. Crack propagation occurred when
the tensile stress due to the increase in suction was equal to or higher
than the cohesion forces. In the untreated samples, as the percentage
of gypsum increases, the percentage of clay in the sample decreases (replacement method) and consequently the shrinkage diminishes. Moreover, gypsum in the soils acts as a ller and participates in the reduction
of suction induced in the clayey parts of the soil. It is worth noting that
after the last wettingdrying cycles most cracks were found to be

0%G

5%G

situated at the same locations as after the rst cycle and the following
cycles enhance only these phenomena. Concerning shrinkage, the dimension can be millimetric and the visible cracks have a homogeneous
distribution and can reach a millimeter.
Figs. 10 and 11 show that the swell potential of the lime-treated soil
samples increased with increasing number of wettingdrying cycles. At
the short-term curing periods (from 2 days to 28 days) and for both
temperature values, the maximum swell potential values were recorded
after the rst wettingdrying cycle. Thereafter, swell values reached
equilibrium or decreased slightly with increasing wettingdrying cycles. Long-term curing periods (more than 28 days) suppressed the
swell potential of the soil samples without gypsum, even with increasing wettingdrying cycles. This behavior is attributed to more cementitious materials being formed during these periods. For the soil samples
containing gypsum, the swell potential values increased with wetting
drying cycles up to the 2nd cycle, then stabilized or decreased slightly.
The results obtained at short-term periods of curing and for both curing
temperatures indicate that the benecial effect of lime treatment is lost
with wettingdrying cycles. These results support the study carried out
by (Khattab et al., 2007). It can be stated that the wettingdrying cycles
caused the gradual destruction of the pozzolanic reaction of limetreated soil samples.
In the treated samples, the claylime reactions are certainly higher
than the suction developed in these soils, which explains why no
shrinkage or cracks were observed.
Moreover, ettringite formation and water absorption also resulted in
increasing the swell potential of the lime-treated soil samples containing gypsum. Swelling in gypseous soil samples is normally associated
with absorption of water during ettringite formation (Hunter, 1988;
Mitchell and Dermatas, 1992). Wild et al. (1993) reported that swelling

15%G

Untreated

180 days at 20C

180 days at 40C


Fig. 9. Crack propagation of soil samples with wettingdrying cycles.

25%G

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

15% G

Free Swell (%)

25% G

2
3
No. of Cycle

2
3
No. of Cycle

0% G

7 days

15% G

5% G
15% G

Free Swell (%)

1.5

25% G

0.5

0% G

7 days

5% G

1.5

Free Swell (%)

15% G

0.5

0.5

25% G

0.5

0
0

2
3
No. of Cycle

2
3
No. of Cycle

28 days

5% G

5% G
15% G

1.5

Free Swell (%)

15% G

1.5

25% G

0% G

0% G

28 days
Free Swell (%)

5% G

1.5

25% G

25% G

0.5

0.5

0
0

2
3
No. of Cycle

0% G
5% G

1.5

180 days

0% G
5% G
15% G

0.5

2
3
No. of Cycle

180 days

15% G

1.5

Free Swell (%)

Free Swell (%)

0% G

2 days

5% G

1.5

Free Swell (%)

0% G

2 days

101

25% G

0.5

25% G

0
0

2
3
No. of Cycle

2
0% G

360 days

0% G

360 days

5% G

1.5

15% G

5% G
15% G

1.5

Free Swell (%)

Free Swell (%)

2
3
No. of Cycle

25% G

0.5

25% G

0.5

0
0

No. of Cycle
Fig. 10. Cyclic free swell of lime treated soil samples cured at 20 C with wettingdrying
cycles.

2
3
No. of Cycle

Fig. 11. Cyclic free swell of lime treated soil samples cured at 40 C with wettingdrying
cycles.

102

A. Aldaood et al. / Applied Clay Science 102 (2014) 93103

conditions and clay content must be made to counter the adverse effects
of lime addition. Such measurements aim to reduce the action of
ettringite formation.

Table 2
Residual water content of lime treated soil with curing conditions.
Gypsum (%)

0
5
15
25
a

Residual water content (%) at 20 C40 C

2 days

7 days

28 days

180 days

360 days

10.39.8
9.89.4
9.69.2
9.59.1

9.69.5
9.39.1
9.19.0
9.08.8

8.67.7
8.07.1
7.56.9
7.26.1

7.46.4
6.75.7
6.25.0
5.94.8

6.85.7
6.15.1
5.54.5
5.14.0

Initial value of water content of all soil samples is = 11%.

in a kaolinitelimegypsum system is related to ettringite formation


and that the swelling increases with an increase in gypsum content
and also increases linearly with water absorption. Generally, there will
be insufcient water to dissolve very much gypsum at the end of the
curing period, especially for long-term periods as shown in Table 2;
moreover, the drying process caused a large reduction in water content
values (water content approximately equal to zero). Thus, unless extra
water is able to enter the soil samples, no appreciable swell will occur,
even if high amounts of gypsum and lime are present. The measured residual water content of lime-treated soil samples decreased with increasing both curing periods and curing temperatures. Further, as
gypsum content increased the residual water content decreased with
curing conditions, as illustrated in Table 2.
Another phenomenon that may help to interpret the increase in
swell potential is that of osmotic suction. During wettingdrying cycles,
water absorption is dominated by osmotic suction which is a function of
gypsum content in the soil samples. The suction potential of soil samples will increase with gypsum movement, resulting in higher water absorption and hence causing an increased swell potential. Lastly, the
lime-treated soil samples did not show any crack propagation during
wettingdrying cycles, as illustrated in Fig. 9.
4. Conclusions
The following conclusions can be drawn from this study.
1. Lime addition and curing conditions (curing periods and curing temperature) enhanced the swell potential of soil samples without
gypsum.
2. In the presence of gypsum and available water, the lime-treated soil
samples show an increase in total pore volume and in swell potential
due to ettringite formation. This distress increases with increasing
curing conditions.
3. Osmotic suction, created by the presence of soluble gypsum in soil
samples, caused additional water absorption and therefore contributed to increasing swell potential. Ettringite nucleation and growth
caused the same action. Changes in the engineering properties and
behavior of soils are due to a set of parameters including gypsum dissolution, pore size distribution and soil fabric changes revealed by
XRD, SEM images and mercury porosimetry tests.
4. The benecial effect of lime treatment in controlling the swell potential of soil samples (especially gypseous soil samples) is partially lost
during wettingdrying cycles. The rst wettingdrying cycle causes
more distress than subsequent cycles for the soil sample with gypsum
content.
5. Based on the results presented in this paper, lime treatment could be
effective in stabilizing gypseous soils containing a small amount of
gypsum (5%), and in enhancing their swell properties, especially
in areas within arid or semi-arid zones.
Finally, provided that precautions are taken to prevent gypsum dissolution, gypseous soils could be carefully used in the liners of sanitary
landlls in those regions where wetdry cycles have a signicant effect
on swelling properties and crack propagation. Further, when gypsum
salts are present in soils and stabilization is required, measurements
such as gypsum content, compaction energy and water content, curing

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