Applied Clay Science 95 (2014) 133–145

Contents lists available at ScienceDirect

Applied Clay Science

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

Research paper

Lime consumption of different clayey soils

Muzahim Al-Mukhtar ⁎, Abdelmadjid Lasledj, J.F. Alcover
CNRS-Université d'Orléans, Centre de recherche sur la matière divisée, 1 bis, rue de la Férollerie, 45071 Orléans Cedex 2, France

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

Article history: This study focused on the lime consumption by 10% of lime treatment, of five soils containing different major clay
Received 15 July 2013 minerals, kaolinite, illite, smectite–kaolinite, smectite–illite and smectite. Assessing the consumption of lime with
Received in revised form 27 March 2014 respect to curing time, using an atomic absorption device, illustrates the lime–clay mineral reaction and the
Accepted 28 March 2014
mechanisms involved in curing in the short- and long-term.
Available online 18 April 2014
X-ray diffraction and thermogravimetric analysis results show that clayey soils have different kinetic reactions
Keywords:
depending on to their mineralogical composition, and that all soils consume the amount of lime added after a
Smectite shorter or longer period of curing time. Two main reactions were assessed: the short-term reaction (cation
Kaolinite and illite exchange and flocculation) and the long-term reaction (pozzolanic reaction). These reactions are initiated due
Lime consumption to the highly alkaline medium induced by the dissolution of lime in the water contained in the soil. The amount
Short-term reaction of lime consumed during the short-term reaction varies from nothing for kaolinite and maximum with sodium-
Pozzolanic reaction smectite. The pozzolanic reaction present in all the clayey soils tested depends on the amount of lime available
Calcium-hydrates and is greatly accelerated by increasing the curing temperature from 20° to 50 °C. This reaction induces structural
and mineralogical changes in the treated soils due to the newly formed calcium hydrates.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction
Lime treatment has a beneficial effect on the properties of clayey
soils by enhancing many of their engineering properties: a reduction
in water content and swelling potential, an improvement in workability
and in-situ compaction, and an increase in mechanical strength
(Al-Mukhtar et al., 2012; Lasledj, 2009; Maubec, 2010; Stoltz et al.,
2012). Lime treatment leads to structural and textural changes in clayey
soils and irreversibly changes their hydro-mechanical behaviour.
The dissolution of lime in the water contained in the treated soil in-
duces a strongly alkaline medium (pH reaching 12.4) and the divalent
calcium cations (Ca++) of lime are dissolved. In the first moments of
the lime treatment, Ca++ fixes to the surface of the clay mineral and
the calcium ions replace most of the available exchangeable cations
(Stumm, 1997). High-valent cations replace lower valent cations and
the larger cations are substituted for smaller ones. Instantaneous
reactions including cation exchange and flocculation–agglomeration
are prompted by the addition of a relatively small amount of lime.
The reaction rate in the long-term depends on only on the crystallo-
graphic nature of the clay minerals (smectite, illite and kaolinite react
differently to the lime effect) but also on the curing temperature
(Little, 1996; Rao and Shivananda, 2005; Rojas and Cabrera, 2002).
When triggered, these long-term reactions enable a further
⁎ Corresponding author. Tel.: +33 2 38 25 78 81; fax: +33 2 38 25 53 76.
E-mail address: muzahim@cnrs-orleans.fr (M. Al-Mukhtar).
improvement in the properties of the treated clayey soil. However this
reaction depends on the presence of a quantity of lime greater than
that used in instantaneous reactions (Eades and Grim, 1960; Hill and
Davidson, 1960; Sivapullaiah et al., 2000). Calcium hydrates (Ca-hy-
drates) formed during the pozzolanic reaction with the silica and alumi-
na released from the clay mineral and the lime (calcium and hydroxyl
ions), are similar to those of hydrated cement (portland): calcium sili-
cate hydrate (CSH) and/or calcium silicate aluminate hydrate (CSAH)
and/or calcium aluminate hydrate (CAH) (Al-Mukhtar et al., 2010a;
Al-Rawas and Goosen, 2006; Arabi and Wild, 1986; Bell, 1996; Board-
man et al., 2001; Diamond and Kinter, 1965; Khattab, 2002). This
crystallisation, although slow at the beginning, will continue as long as
residual calcium is available and the pH is high enough. The kinetics of
the pozzolanic reaction depend on several factors, including the physi-
cal and chemical characteristics of the treated clay mineral, curing tem-
perature, moisture and freeze–thaw cycles (Al-Mukhtar et al., 2010b;
Khattab et al., 2007; Liu et al., 2010; Rao and Shivananda, 2005).
The aim of this work was to study the mechanisms involved in the
clay mineral–lime reaction in both the short-term and long-term by
monitoring the progress of lime consumption during six months,
using atomic absorption, for two curing temperatures of 20 °C and
50 °C. Five different clayey soils with different mineralogical composi-
tions of Na+-smectite, Ca++–Mg++ smectite, illite and kaolinite were
studied. A high amount of lime addition (10%) was used in this study
to ensure a complete reaction with the soils and to easily determine
the amount of lime consumed by the clayey soils tested. Changes in

http://dx.doi.org/10.1016/j.clay.2014.03.024
0169-1317/© 2014 Elsevier B.V. All rights reserved.
134 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145

the mineralogy of the five clayey soils due to lime treatment were Table 2
studied by X-ray diffraction (XRD) and thermogravimetric analysis Mineralogical composition (mass%) of the clayey soils tested.

(TGA). The mineralogical changes and the assessment of lime consump- Clayey soils/ Kaol soil I soil Sm–Kaol soil Sm–I soil Sm soil
tion lead to a better understanding of the main factors that control the components
progress (kinetics) of lime–clay reactions. Smectite – – 48.0 38.1 72.0
Illite 10.0 55.0 – 40.0 15.0
2. Materials and methods Kaolinite 83.0 22.0 38.0 – 10.0
Quartz 7.0 9.0 3.2 10.6 0.8
Calcite 0.0 13.0 3.4 10.3 2.1
2.1. Materials Goethite 0.0 0.0 6.4 0.0 0.0
Anatase 0.0 0.1 1.0 0.9 0.1
The main clay minerals of the five clayey soils tested are kaolinite, Exchange – – Na+ Ca++, Mg++ Ca++, Mg++
illite, smectite/kaolinite, smectite/illite and smectite. These soils have cation
Main mineral Kaolinite Illite Smectite kaolinite Smectite illite Smectite
different pH, electrical conductivities (EC) and cation exchangeable ca-
pacities (CEC), and are denoted as Kaol, I, Sm–Kaol, Sm–I and Sm respec-
tively. The chemical and the mineralogical compositions of these soils containing 50 mL (50 g) of demineralised water then the bottle was
are given in Tables 1 and 2. closed. The mixture was protected from the atmosphere to avoid car-
Kaol soil contains 83% kaolinite and the rest is composed of 10% illite bonation of the lime during curing. The mixture was periodically stirred
and 7% quartz. The major component of I soil is illite (55%). The Sm–Kaol to ensure uniformity until the end of the curing time, at which time the
soil is a mix of 48% dioctahedral Na+-smectite (with sodium as the main test solution was extracted, filtered to 0.45 μm and analysed.
exchangeable cation) and 38% kaolinite. An equivalent percentage of
smectite and illite compose the Sm–I soil, with two exchangeable
cations: Ca++ and Mg++. In the Sm soil, the percentage of smectite is 2.2.2. Determination of mineralogical changes by XRD and TGA
about 72% with exchange cations Ca++ and Mg++. These soils with dif- The mineralogical changes were studied by XRD and TGA performed
ferent mineralogical compositions and properties (CEC and swelling) on the samples treated and compacted after a long curing period
were chosen to represent different types of clay minerals: interlayer (6 months) at 20 and 50 °C. At the end of the curing time and before
space with exchangeable cations (smectite), and interlayer space with- testing the samples were dried for 4 h in an oven at 50 °C, ground,
out exchangeable cations (kaolinite, illite); layers with a TO structure, and then sieved at 100 μm.
i.e. one tetrahedral (T) sheet and one octahedral (O) sheet, that is re- XRD was performed on the powder, using CuKα1 radiation, obtained
peated (kaolinite) and layers with a TOT structure, i.e. one octahedral with a monochromator. The diagrams were recorded on a Philips
(O) sheet between two tetrahedral (T) sheets that is repeated (smectite, PW3020 diffractometer (scanning from 2° to 70° with a step width of
illite) (Bergaya and Lagaly, 2006). 0.1° and time step of about 100 s).
A commercial hydrated lime (Calcia) was used for treatment of the TGA was performed using a Setaram TGA 92 apparatus. Samples
studied soils. This commercial lime contains 94% lime (portlandite) — were first dried in a desiccator with P2O5 to stabilise the mass of the
Ca(OH)2 — and 6% calcite. sample. The heating rate was 1.7 °C/min under an argon flow. The
temperature varied from 20 °C to a final temperature of 900 °C, with a
2.2. Methods plateau (fixed temperature) at 110 °C for 2 h. The stand-by at 110 °C
led to a constant mass in time at this temperature, which served as
2.2.1. Determination of lime consumption by chemical analysis the reference mass.
The determination of lime which has not reacted with the clay min-
eral was carried out by atomic absorption spectrometry (AAS) using a
Hitachi Z-8100 Polarized Zeeman device. The concentration of calcium 3. Results and analyses
was measured in the solutions extracted from mixtures of lime-
treated soil, after curing times of 1.5 h, 7 days, 28 days, and 3 months 3.1. Lime consumption
and 6 months and for two curing temperatures of 20 and 50 °C. The
lime consumption was deduced from these measurements. It must be mentioned here that the maximum amount of lime that
Samples of treated soil were prepared by mixing 0.5 g soil with 2, 4, can be consumed is 9.4%, since the lime added contained 6% calcite
6 and 10% lime. The lime–soil mixture was dispersed in a bottle and 94% lime.

Table 1
Lime consumed after 1.5 hour (%)

Chemical composition, pH, electrical conductivity (EC) and cation exchange capacity
6
Sm-Kaol soil
(CEC) of the clayey soils tested.
Sm soil
5
Clayey soils element Kaol soil I soil Sm–Kaol soil Sm–I soil Sm soil Sm-I soil
I soil
SiO2 48.0 49.7 46.0 55.0 55.8 4 Kaol soil
Al2O3 36.5 15.8 23.3 15.5 18.0
Fe2O3 0.9 6.0 7.6 5.4 4.4
MnO Trace 0.1 0.1 0.0 0.0 3
MgO 0.2 2.5 1.4 2.1 5.9
CaO 0.2 8.9 4.4 8.9 3.4 2
Na2O 0.1 0.1 2.5 0.2 0.1
K2O 1.4 3.9 0.2 2.9 1.2
TiO2 0.2 0.8 1.0 0.8 0.4
1
P2O5 0.0 0.1 0.0 0.0 0.0
Loss on ignition 12.5 12.0 12.3 9.2 10.4 0
pH 6 7.4 10.6 7.9 8.1 0 2 4 6 8 10 12
EC, mS/cm - 1.9 2.7 2.3 2.3 Lime added (%)
CEC, meq/100 g of soil 3–15 10–40 70–120
(Bergaya et al., 2006)
Fig. 1. Immediate lime consumed (1.5 h) by different clayey soils tested.
 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 135

3.1.1. Immediate lime consumption with added lime
The immediate measurements of lime consumption (Fig. 1) were
carried out at 20 °C, one and a half hours after treatment of the soil
with lime (2%, 4%, 6% and 10%). The results clearly indicate that the
instantaneous reaction between the lime and clay mineral is governed
by cation exchange: very significant lime consumption for the Sm–
Kaol soil (replacement of sodium cations in the interlayer space of the
smectite layers by calcium cations) and negligible lime consumption
for the Kaol soil. For the other three soils, lime consumption varied be-
tween values obtained for the Sm–Kaol soil (5.1%) and Kaol soil (0%):
4.9% for the Sm soil, 3.9% for the Sm–I soil (smectites with Ca++ and
Mg++ as exchangeable cations), and 1.1% for the I soil (illite). About
5% of lime seems to be the maximum quantity consumed in the short-
term at 20 °C by the Sm soils.
3.1.2. Lime consumption with curing time
The assessment of 10% lime consumption with curing time at 20 °C
and 50 °C (Fig. 2a and b) shows that lime continues to be consumed
with curing time due to the pozzolanic reaction following the immedi-
ate lime consumption (i.e. cation exchange reaction).
Lime reactions with the clay mineral lead to the formation of new
Ca-hydrates (CSH, CAH, CSAH). These reactions involve the slow con-
sumption of lime at 20 °C and fast (accelerated) lime consumption at
50 °C with curing time. For all the tested soils, lime needed more than
a tion of the soil. The pozzolanic reaction develops with the destruction
Lime consumed during curing at 20°C (%)
3 months to be consumed when the curing temperature was 20 °C
(Fig. 2a), while for all the tested soils cured at 50 °C, except the Kaol
soil, practically the entire amount of lime added (9.4%) was consumed
within one month (Fig. 2b). The different lime consumption rates
reached in 7 days at 50 °C and in 28 days at 20 °C (Table 3) are attribut-
ed to the start of the pozzolanic reaction. At a curing temperature of
20 °C, the rate (kinetics) of lime consumption is similar for the three
clayey soils containing smectite (0.08–0.07 lime%/day), lower for the I
soil (0.06 lime%/day) and the lowest value was found for the Kaol soil
(0.04 lime%/day). At a curing temperature of 50 °C, the results demon-
strate that the kinetics of lime consumption is quite similar for the test-
ed clayey soils but slowest for the Kaol soil. In the initial days of
treatment, the lime consumption at 50 °C compared to 20 °C curing
can increase 13-fold for the I soil, 6-fold for the Kaol soil and 5–7 fold
for the other three soils containing smectite. Rojas and Cabrera (2002)
and Al-Mukhtar et al. (2010b) reported similar results concerning the
kinetics of the lime–clay mineral reaction with curing temperature.
The rate of many chemical reactions and certain physical processes
increase exponentially with temperature and can be described by the
Arrhenius equation. Therefore, increases in lime consumption with
temperature are assumed to follow the simple law of Arrhenius-type
behaviour. The chemical activation energy (Ea) calculated in Table 3
for the lime consumption of the tested soils (activation energy related
to the pozzolanic reaction) is about 44 kJ/mol for the Kaol soil; about
63 kJ/mol for the I soil and about 40–47 kJ/mol for the Sm, Sm–Kaol
and Sm–I soils. These different lime consumption increases and activa-
tion energies demonstrate the influence of the mineralogical composi-

of the clay mineral silicate layer and the formation of Ca-hydrates

such as CSH, CAH and CSAH.
10 This behaviour can be explained by the structure of the different clay
% of lime added
minerals tested (Bergaya et al., 2006; Grim, 1962; Ingles and Metcalf,
8 1972; Konan et al., 2007). Illite and smectite have nearly the same TOT
layer, the main difference is being in the interlayer space: an interlayer
space with exchangeable cations (Na+, Ca++ or Mg++ and nH2O) in
6
smectite, or an interlayer space without easily exchangeable cations
(K+) in illite. The difference in swelling property and CEC between
4 smectite and illite explains the difference observed in the activation en-
Sm-Kaol soil
Sm soil
ergy, 40 and 63 kJ/mol respectively, as the opening of the silicate layer
2 Sm-I soil (needed for the pozzolanic reaction) is more difficult in illite than smec-
I soil tite. Kaolinite has a TO layer and no interlayer cations; these parameters
Kaol soil
explain the slow kinetics of the pozzolanic reaction.
0
0 50 100 150 200 Moreover, as mentioned during the short time reaction (after 1.5 h
Curing time (day) of treatment with 10% lime), the non-consumed lime available for the
pozzolanic reaction is about 5% for the Sm and Sm–Kaol soils, 6% for
the Sm–I soil, 9% for the I soil and 10% for the Kaol soil. Al-Mukhtar
b et al. (2010a,b) demonstrated that in a clayey soil, at 20 °C and 50 °C,
Lime consumed during curing at 50°C (%)

as the amount of available lime increases the initial rate of lime

10 % of lime added
consumption increases, and the newly-formed Ca-hydrates due to the
pozzolanic reaction increase. Nevertheless, at 20 °C after 6 months of
8 curing time, illite and kaolinite with more lime available consume less
lime than smectite. Therefore, the nature of the clay mineral is more sig-
nificant than the amount of non-consumed lime available at the end of a
6 short-time reaction.
Sm-Kaol soil Over time, the lime consumption continues for all the clayey soils
4 Sm soil tested due to the development of the pozzolanic reaction, which con-
Sm-I soil sumes the lime and induces the formation of new Ca-hydrates, as con-
I soil
firmed by XRD and TGA analysis.
2
Kaol soil

3.2. Mineralogical composition of untreated and lime-treated clayey soils as

0
0 50 100 150 200 detected by XRD
Curing time (day)
XRD patterns of the five studied soils, both untreated and 10% lime-
Fig. 2. Lime consumption for the clayey soils tested with curing time at 20 °C (a) and 50 °C treated, after at least 6 months of curing at 20 °C and 50 °C are present-
(b). ed in Figs. 3–7.
136 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145

Table 3
Average lime consumption rate by lime treated soils, cured at 20 °C and 50 °C.

Average lime consumption rate (LCR) at T°C in lime mass percentage/day Clayey soils

Kaol soil I soil Sm–Kaol soil Sm–I soil S soil

LCR at T2 = 20 °C during the first month 0.04 0.06 0.08 0.07 0.075
LCR at T1 = 50 °C during the first week 0.24 0.78 0.46 0.48 0.39
Rate ratio [LCR 50 °C/LCR 20 °C] = k 6 13 5.8 6.8 5.2
Activation energy (Ea) (kJ/mol) 44 63 43 47 40

LCR = k(T) = A · exp(−Ea / RT) and Ea(T1 − T2) = R · T1 · T2 · [Ln k(T1) − Ln k(T2)].
Activation energy (kJ/mol) = 8.32 · 10−3 · 293 · 323 · Ln [LCR50 °C / LCR20 °C] / 30 = 24.5 · Ln k.

3.2.1. Mineralogical composition of untreated tested clayey soils weak basal 00ℓ reflections and the large two-dimensional {h,k} band
The diffractograms of the untreated clayey soils (Figs. 3–7) show re- reflections, indicate that Sm–Kaol, I, Sm–I and S soils are formed of
flections of clay minerals: smectite (Sm), kaolinite (Kaol), illite (I) and of particles of a few clay mineral layers, and are randomly stacked.
non-clay minerals: quartz (Q), goethite (G), calcite (C) and anatase (An)
in different concentrations. On these figures, reflections characteristic of 3.2.2. Mineralogical changes in lime-treated clayey soils
clay minerals are observed:
3.2.2.1. Kaol soil. The two diffractograms (Fig. 3) of the lime-treated Kaol
– 00ℓ basal reflections due to stacking of clay mineral layers, in partic-
soil (83% kaolinite and 10% illite) show three new reflections at 2θ =
ular the (001) reflection, which are generally large.
11.6°, 23.6° and 31.3° (0.76, 0.376 and 0.286 nm). These reflections cor-
– {hkℓ} reflections due to the two-dimensional hexagonal structure of
respond to a calcium aluminate hydrate (CAH) of the form Ca3Al2O6,
the clay mineral layers (TO or TOT), mainly the first reflections {02ℓ}
xH2O (02-0083, JCPDS — Joint Committee on Powder Diffraction Stan-
{11ℓ}.
dards). This new mineral is formed by the pozzolanic reaction between
XRD shows that the Kaol soil (Fig. 3) is a well-ordered kaolinite with the lime and clay minerals. The intensity of these reflections increases
high intensities and thin basal 00ℓ reflections of diffraction which with temperature. The reaction rate increases with curing temperature
means there are many stacked clay mineral layers; two-dimensional and leads to more significant CAH formation.
{h,k,ℓ} bands with closely-spaced but separate 02ℓ and 11ℓ signifies The diffractogram at 50 °C shows the emergence of two new reflec-
an ordered stacking of the layers. tions with a very low intensity at 2θ = 7.0° and 14.1° (1.26 nm and
In contrast, XRD shows that the clay minerals of the Sm–Kaol soil 0.63 nm). These reflections can be attributed to a calcium silicate alumi-
(Fig. 4) are poorly organised: only one broad 001 reflection of smectite nate hydrate (CSAH) of the form Ca2Al2SiO7, 8H2O (30-0227, JCPDS).
and kaolinite which means very few assembled layers; and relatively The formation of CSAH induced by the pozzolanic reaction is very
high and asymmetric {h,k} bands for (02,11); (20,13) which signifies slow, even at 50 °C.
many disoriented particles with large ab faces that are randomly The presence of reflections of the lime on treated Kaol soil at 20 °C
stacked. indicates that not all the added lime has been consumed after 6 months
Sm–Kaol soil is a mix of Na+-smectite and kaolinite. I soil (Fig. 5) is of curing, in contrast with the treated Kaol soil at 50 °C. These results are
largely composed of illite with some kaolinite, quartz and calcite. Sm–I consistent with those of lime consumption at 20 °C (Fig. 2a) and at
soil (Fig. 6) is composed of a mix of illite and smectite, with quartz 50 °C (Fig. 2b). The XRD patterns of the treated Kaol soil indicate the ap-
and calcite. Sm soil (Fig. 7) is mainly composed of smectite, with a pearance of the main reflection of calcite at 2θ = 29.45°, resulting from
small amount of illite, kaolinite, calcite and quartz. The broad and the calcite that is included as an impurity in the added lime. This calcite

1000
Kaol soil
K 001
Intensity -arbitrary units ( counts/s )

K 002

800
Quartz
CAH

Calcite
CAH

CAH
CSAH

Lime treated soil after

6 months at 50°C
600
CSAH

Lime
Lime

400 Lime treated soil after

6 months at 20°C
Il 001

200
Quartz
Il 002

Il 005

K 004

K-I
Il 006

33,06

K-I Untreated
02 ,11 20 ,13 soil
0
0 10 20 30 40 05 60 70
2θ (°)

Fig. 3. X-ray diffraction results of untreated and lime treated Kaol soil.
 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 137

500
Sm-Kaol soil

CSH or CSAH
Intensity -arbitrary units (counts/s)
400

Lime treated soil after

CAH
CAH
12 months at 50°C

300

200 Lime treated soil after

CAH

CAH
6 months at 20°C

Quartz, Q
Calcite, C

S-K 02 ,11
100

Anatase An
S001

C+Q
S-K 02 ,11

S-K 33,06
Goethite G
Q

C
G
K001

Untreated

C
soil

C
G

G
Q

Q
0
0 10 20 30 40 50 60 70
θ (°)
2θ

Fig. 4. X-ray diffraction results of untreated and lime treated Sm–Kaol soil.

could also be due to the partial carbonation of lime by CO2 in the atmo- Moreover, XRD patterns of the lime-treated Sm–Kaol soil after
sphere during mixing. 6 months of curing at 20 and 50 °C indicate that:

– no lime reflections are observed. This proves the complete consump-

3.2.2.2. Sm–Kaol soil. Diffractograms (Fig. 4) of the lime-treated Sm–Kaol tion of lime as revealed by chemical analysis (Fig. 2). In contrast, in
soil (48% Na+ smectite and 38% kaolinite) at 20 °C and 50 °C show the the treated Kaol soil cured at 20 °C, after 6 months the lime con-
appearance of reflections at 2θ = 11.6° (0.76 nm) and at 2θ = sumption is not complete.
23.6°(0.376 nm) of the same CAH of the form Ca3Al2O6, xH2O (02- – a small increase in the intensity in the calcite reflections, induced by
0083, JCPDS). The intensity of the CAH reflections decreases slightly the impurity of the added lime and the partial carbonation of the
with an increasing temperature from 20 °C to 50 °C, while the rate of lime by CO2 in the atmosphere during mixing.
the reaction increases with temperature. This behaviour can be attribut- – a decrease, mainly at 50 °C, in the intensity of the reflection charac-
ed to the development of other Ca-hydrates with temperature. teristics of the clay layers {smectite and kaolinite two-dimensional
The diffractogram of this treated soil cured at 50 °C also shows the band reflections (02,11), (20,13) and (33,06)}, which reflects the de-
appearance of a shoulder at 2θ = 29° (0.308 nm) on the main reflection struction of the clay layers.
of calcite at 2θ = 29.45° (0.3035 nm). This broadening may correspond
to a reflection of a CSH of the form, Ca3Si2O7, xH2O (33-0306, JCPDS) or
CSAH of the form Ca3Al2SiO4(OH)8 (38-0368 and 32-0151, JCPDS). This 3.2.2.3. I soil, Sm–I soil and Sm soil. The diffractograms (Fig. 5) of the I soil
enlargement is also visible but weaker on the diffractogram of the soil (55% illite and 22% kaolinite) treated with 10% lime at 20 and 50 °C for
treated at 20 °C. 6 months of maturation show the appearance of the main reflection

500
I soil
Quartz
Intensity -arbitrary units ( counts/s)

400

Lime treated soil after

6 months at 50°C

300
Calcite, C
Quartz, Q

Lime

200 Lime treated soil after

CAH

6 months at 20°C

100
02 ,11

20 ,13
Il 001

Untreated
Q+C
Q

33,06
K 001

Il 002

soil
Q
Q
C

C
Q

C
C

Q
Q
Q

0
0 10 20 30 40 50 60 70
2θ (°)

Fig. 5. X-ray diffraction results of untreated and lime treated I soil.

138 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145

500
Sm-I soil

Intensity -arbitrary units (counts/s)

400

Lime treated soil after

6 months at 50°C

300

Quartz, Q

Calcite, C
200 Lime treated soil after
6 months at 20°C

100

S-I 02 ,11

S-I 20 ,13
S 001

Untreated

S-I 33,60
Il 001

Q+C
Q
soil
Il 002

Q
Q
C

Q
C

Q
C

C
Q

Q
Q

C
0
0 10 20 30 40 50 60 70
θ (°)
2θ

Fig. 6. X-ray diffraction results of untreated and lime treated Sm–I soil.

corresponding to CAH already observed in the Sm–Kaol and Kaol soils images for a Sm–Kaol soil that the growth of Ca-hydrates begins near
treated under the same conditions. or on the clay layer surfaces. The smectite is not well ordered as in kao-
As in the Kaol soil, a weak lime reflection is still observed in the sam- linite or illite, and its surface resembles a large soft and thin sheet.
ple cured at 20 °C for six months, and lime consumption is not complete Therefore the growth of well-crystallised Ca-hydrates is not promoted
(Fig. 2a); all the added lime is only consumed at 50 °C (Fig. 2b). More- on the surface of the Sm soil which explains the lack of XRD reflections.
over, as in the Sm–Kaol soil, the intensity of the CAH reflection decreases
slightly with increasing temperature from 20 °C to 50 °C. This behav- 3.3. TGA of untreated and treated clayey soils
iour can be attributed to the existence of other pozzolanic reactions.
Such competing reactions can result in other Ca-hydrates at higher For temperatures higher than 110 °C, the thermogravimetric curves
temperatures. (TG) and their derivatives (DTG), of the five soils, both untreated and
The diffractograms (Fig. 6) of the Sm–I soil (40% illite and 38% Ca++, 10% lime-treated for 6 months at 20 °C and 50 °C are presented in
Mg++smectite) and the diffractograms (Fig. 7) of the Sm soil (72% Figs. 8–12. The relative loss in mass (TG) is defined by:
Ca++, Mg++smectite, 15% illite and 10% kaolinite) treated with 10%
lime at 20 and 50 °C for 6 months show no new reflections. The lack TGðTÞ ¼ ½MðTÞ−MðT0 Þ=MðT0 Þ ð1Þ
of XRD observations of calcium hydrates — even though the lime was
with:
completely and quickly consumed at 20 °C — can be interpreted by
the formation of a compound in an amorphous state or by weakly- – M(T0) as the reference mass at T0 = 110 °C.
developed crystallisation. Lasledj (2009) demonstrated with TEM – M(T) as the mass at the applied temperature T.

500
Sm soil
S 001
Intensity -arbitrary units (counts/s )

400

Lime treated soil after

6 months at 50°C

300

200 Lime treated soil after

6 months at 20°C
S-I 02 ,11

S-I 15 ,24 ,31

100
S-I 20 ,13
Calcite, C
Quartz, Q

S-I 33,06

Untreated
Il 001

K 001

Il 002

soil

0
0 10 20 30 40 50 60 70
2θ (°)

Fig. 7. X-ray diffraction results of untreated and lime treated Sm soil.

 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 139

Temperature (°C)
100 200 300 400 500 600 700 800 900
0
Lime
-2

-4
Lime
-6 Untreated Kaol soil
TG (%)
Treated Kaol soil after 6 months at 20°C
Treated Kaol soil after 6 months at 50°C
-8

-10

-12

-14
Interlayer water and New Ca-hydrates Kaolinite ........... Illite Calcite

-16
Temperature (°C)
100 200 300 400 500 600 700 800 900
0

-0,04
Interlayer water and New Ca-hydrates Lime
Calcite
DTG (%/min)

-0,08 Illite

-0,12

-0,16
Untreated Kaol soil
Treated Kaol soil after 6 months at 20°C
-0,2 Treated Kaol soil after 6 months at 50°C

Kaolinite
-0,24

Fig. 8. Thermogravimetric analysis of untreated and lime treated Kaol soil.

The TG and DTG curves provide a comparison between untreated
and treated samples, which initially had the same proportion of clay
mineral (90% of the total mass, M(T0)) and show the effect of the
treatment:
– It allows the estimation of the relative loss in mass due to the linked
water of the interlayer space of the smectite; dehydration of the Ca-
hydrates formed due to the pozzolanic reaction between 110 and
400–500 °C.
– It also identifies the mass loss due to the dehydroxylation of kaolin-
ite (between about 400 and 550 °C), smectite and illite (between
500 and 650 °C).
– The final peak between 600–650 °C and 700–750 °C is related to the
decarbonation of calcite (a mineralogical component of the soil,
added with the lime, and possibly formed by the carbonation of
lime during curing).
3.3.1. TGA analysis of Kaol soil
TG and DTG curves for the untreated and lime-treated Kaol soil after
6 months of curing at 20 and 50 °C are compared (Fig. 8) for samples
initially containing 90% Kaol soil and 10% lime. The TG curve of 10% of
the lime sample is also presented in Fig. 8.
Lime treatment modifies the structure of the Kaol soil as shown by
the differences between the TG and DTG curves of the untreated and
the lime-treated Kaol soil.
The TG curves of the untreated soil and treated soil are very different,
mainly between 110 and 400 °C. In fact, between 110 and 400 °C the
mass losses are practically negligible in the untreated Kaol soil; while
in the two treated Kaol soils the mass losses increase almost continu-
ously with temperature and correspond to the broad band observed in
the DTG curves of the treated samples cured at 20 °C and 50 °C. These
losses in mass (2.2% at 20 °C and 3.7% at 50 °C) can be attributed to
the dehydration of the new Ca-hydrates formed by the pozzolanic reac-
tion and detected by XRD (Fig. 3). The broad band can also be attributed
to the dehydration of a kaolinite layer, partially damaged by lime treat-
ment. The pozzolanic reaction is more advanced at 50 °C than at 20 °C,
which may explain the lower loss in mass at 20 °C.
The DTG curves of the untreated soil and of the treated samples
show a large endothermic peak at 500 °C due to the dehydroxylation
of kaolinite. The asymmetry of the kaolinite peak toward higher tem-
peratures is due to the dehydroxylation of illite at about 600 °C. The
DTG curves of the treated samples show a decrease in the kaolinite
peak at 500 °C, attributed to the partial destruction of the clay layer.
The proportions of kaolinite measured between 400 and 600 °C slightly
decrease in the treated Kaol soil, where 5 and 7% of the kaolinite is
140 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145

Temperature (°C)
100 200 300 400 500 600 700 800 900
0

-2 Untreated Sm-Kaol soil

Treated Sm-Kaol soil after 6 month at 20°C

-4 Treated Sm-Kaol soil after 6 months at 50°C

-6
TG (%)

-8

-10

-12

-14
Inter-layer water , Goethite and Ca-hydrates Kaolinite Smectite Calcite
-16

Temperature (°C)
100 200 300 400 500 600 700 800 900

-0,01

-0,04
Smectite
DTG (%/min)

Goethite

-0,07
Inter-layer water and Ca-hydrate

Calcite

-0,1
Kaolinite

Untreated Sm-Kaol soil

-0,13 Treated Sm-Kaol soil after 6 months at 20°C

Treated Sm-Kaol soil after 6 months at 50°C

-0,16

Fig. 9. Thermogravimetric analysis of untreated and lime treated Sm–Kaol soil.

destroyed by treatment at 20 and 50 °C, respectively. The very small
amount of illite in the clayey soil does not permit observations of its in-
fluence during treatment.
The DTG curve of the sample cured at 20 °C has two endothermic
peaks: the first peak at 400 °C due to the dehydration of the non-
consumed lime and the second peak at 650 °C due to the decarbonation
of calcite. There is a significant increase in the mass loss of calcite. This
calcite is an impurity of the lime (6% calcite in the added lime) and
comes from the carbonation of lime (calcite is formed during the mix-
ture and curing of the lime–soil due to the reaction of CO2, in the air,
with the lime).
The DTG curve of the sample cured at 50 °C, compared to that of the
sample cured at 20 °C, shows an increase in the mass loss between 110
and 400 °C and the appearance of a peak at 280 °C. This higher loss in
mass can be attributed to the dehydration of a larger amount of CAH
formed by the pozzolanic reaction, as shown by XRD (Fig. 3). The peak
at 280 °C can be attributed to the dehydration of the CSAH observed by
XRD. The DTG curve also shows the disappearance of the peak at
400 °C (all the added lime is consumed by the pozzolanic reaction after
6 months at 50 °C, which confirms the XRD analysis), and the quasi-
disappearance of the peak at 650 °C (the calcite detected is very low).
Comparing the sample cured at 20 °C and that at 50 °C demonstrates
that the lime is consumed faster at 50 °C than at 20 °C, and that calcite
formation by lime and atmospheric CO2 is less significant since the poz-
zolanic reaction is more active at a temperature of 50 °C.
3.3.2. TGA analysis of Sm–K soil
TG and DTG curves for the untreated and lime-treated Sm–K soils
after 6 months of curing at 20 and 50 °C (Fig. 9) are similar, indicating
the close mineralogical compositions of the samples. As with the Kaol
soil, the TG curves of the untreated soil and treated soil are mainly dif-
ferent between 110 and 400–450 °C. The TG curves of the untreated
and lime-treated Sm–Kaol soil show a continuous increasing loss in
mass up to 400 °C, with a higher increasing loss for the treated samples.
For the untreated soil, the DTG shows a large band between 110 and
350–400 °C, which corresponds to a continuous departure of water
linked to interlayer smectite cations (Na+). The DTG curves of the treat-
ed samples reveal a new endothermic peak between 110 and 250 °C.
This peak can be attributed to dehydration of a new Ca-hydrate (CAH)
formed by the pozzolanic reaction and detected by XRD (Fig. 4). The
presence of water and/or Ca-hydrates is much greater in the treated
 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 141

Temperature (°C)
100 200 300 400 500 600 700 800 900
0
Untreated I soil
-2 Treated I soil after 6 months at 20°C

Treated I soil after 6 months at 50°C

-4

-6
TG (%)

-8

-10

-12

-14
Interlayer water and Ca-hydrates Kaolinite Illite Calcite
-16

Temperature (°C)
100 200 300 400 500 600 700 800 900
0

-0,03

-0,06
Interlayer water and Ca-hydrates Kaolinite Illite
DTG (%/min)

-0,09

-0,12

-0,15
Untreated I soil

-0,18 Treated I soil after 6 months at 20°C

Calcite
Treated I soil after 6 months at 50°C
-0,21

-0,24

Fig. 10. Thermogravimetric analysis of untreated soil and lime treated I soil.

Sm–Kaol sol (5%) than in the untreated soil (2.1%), and it increases
slightly with curing temperature (5.0% at 20 °C and 5.4% at 50 °C).
The peak located between 260 and 320 °C corresponds to the dehy-
dration of goethite (transformation of goethite FeO(OH) to hematite
Fe2O3).
The dehydroxylation of clay minerals occurs between 400 °C and
650 °C, where in the DTG curves the peak between 400 and 500 °C is re-
lated to the departure of kaolinite structural water and the band from
500 to 650 °C is related to smectite structural water. The dehydroxyl-
ation of kaolinite and smectite is lower in the treated samples; this
decrease in mass losses is attributed to the partial destruction of the
clay layers, induced by the lime treatment. The proportion of destroyed
kaolinite is higher at 50 °C (28%) than at 20 °C (20%), as for destroyed
smectite (14%) at 50 °C and (10%) at 20 °C.
The final peak between 650 °C and 730 °C is related to the decarbon-
ation of calcite. Calcite is a mineralogical component of the Sm–Kaol soil
(3.4% was detected in the mineralogical composition) and comes from
the added lime. Furthermore, calcite is formed by the carbonation of
lime during curing, in particular at 20 °C. The departure of CO2 is shifted
toward higher temperatures, as the amount of calcite in this soil
increases and the heating rate is too fast. Finally, at 50 °C the pozzolanic
reaction is more advanced than at 20 °C, which may explain the slightly
higher Ca-hydrate formation and clay mineral destruction.
3.3.3. TGA analysis of I soil, Sm–I soil and Sm soil
TG and DTG curves for untreated and treated I soil, Sm–I soil and Sm
soil after 6 months of curing at 20 and 50 °C are presented in
Figs. 10–12. TGA curves for these clayey soils show, as for the Kaol and
Sm–Kaol soils, a strong and continuous increase in mass loss between
110 and 400 °C, and even up to 500 °C for the Sm soil. This behaviour
can be attributed to the dehydration of Ca-hydrates formed by the poz-
zolanic reaction in the treated clayey soils. The amount of interlayer
water in the untreated illite soils is lower than in the smectite soils,
and there is no water in the interlayer of the kaolinite soil. For Sm–I
and Sm soils there is a slight decrease in mass losses due to the dehy-
droxylation of smectite at about 500–600 °C, attributed to the partial
destruction of the clay layers. Between 650 °C and 730 °C, as for the
other tested soils, there is an increase in the decarbonation of calcite.
The DTG curves confirm the composition of these different clayey soils
and the newly formed Ca-hydrates in the lime-treated samples. The
142 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145

Temperature (°C)
100 200 300 400 500 600 700 800 900
0
Untreated Sm-I soil

-2 Treated Sm-I soil after 6 months at 20°C

Treated Sm-I soil after 6 months at 50°C

-4

-6
TG (%)

-8

-10

-12

-14
Interlayer water and Ca-hydrates Smectite Illite Calcite
-16

Temperature (°C)
100 200 300 400 500 600 700 800 900

-0,03
Interlayer water and Ca-hydrates Smectite Illite
DTG, %/min

-0,06

-0,09

Untreated Sm-I soil

-0,12 Treated Sm-I soil after 6 months at 20°C

Treated Sm-I soil after 6 months at 50°C

Calcite

-0,15

Fig. 11. Thermogravimetric analysis of untreated and lime treated Sm–I soil.

TGA curves also indicate that the amount of new Ca-hydrates formed by
lime treatment is less significant in illite soils than in the kaolinite and
smectite soils.
3.3.4. Discussion
To analyse the effect of 10% lime treatment on the five clayey soils
cured at 20 and 50 °C, the following results are summarised in Table 4:
– the proportions of lime consumed after 1 month and 6 months of
curing measured by AAS;
– the proportions of clay mineral destroyed by lime treatment after
6 months of curing determined by TGA;
– the proportions of new Ca-hydrates formed after 6 months of curing
determined by TGA.
At 20 °C of curing temperature, after one month, for the five clayey
soils the added lime is partially consumed; 63–79% for the three smec-
tite soils, 31% for illite and 13% for kaolinite. These proportions of lime
consumed increase with curing time, and after 6 months reach 100%
lime added for the tested smectite soils, 83% for illite soil and 44% for ka-
olinite soil. At 50 °C of curing temperature and after 1 month, the lime
consumptions are: for smectite soils, 91–98%, for illite soil, 88% and for
kaolinite soil, 68%. After 6 months all the added lime has been con-
sumed in the five soils tested.
The pozzolanic reaction which develops with the lime consumption
is very slow in the kaolinite (Zhou and Gunter, 1992) and illite soils. The
faster lime consumption by smectite can be attributed in part to its cat-
ion exchange capacity and to its soft structure (large and thin TOT
layer). K+, the illite interlayer cation, is very difficult to exchange and
theoretically kaolinite has no CEC, so the layers of illite (TOT) and kao-
linite (TO) are not easily opened (Bergaya et al., 2006). Therefore the
proportions of lime available after short-term reactions are higher for
kaolinite and illite than for smectites.
TGA enables estimation of the proportion of clay mineral destroyed
due to lime treatment by studying the dehydroxylation of kaolinite be-
tween 400 and 500 °C and that of smectite and illite between 500 and
650 °C. The proportion of kaolinite destroyed after 6 months at 20 °C
and 50 °C is greater in the Sm–Kaol soil (20–28%) and Kaol soil
 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 143

Temperature (°C)
100 200 300 400 500 600 700 800 900
0
Untreated Sm soil

-2 Treated Sm soil after 6 months at 20°C

Treated Sm soil after 6 months à 50°C

-4

-6
TG (%)

-8

-10

-12

Interlayer water and Ca-hydrates Kaolinite Smectite and Illite Calcite

-14

Temperature (°C)
100 200 300 400 500 600 700 800 900

0
Kaolinite

-0,03
DTG (%/min)

Smectite Illite

Inter-layer water and Ca-hydrates

-0,06

Calcite

Untreated Sm soil
-0,09
Treated Sm soil after 6 months at 50°C
Treated Sm soil after 6 months at 20°C

-0,12

Fig. 12. Thermogravimetric analysis of untreated and lime treated Sm soil.

(5–7%) than in the other tested soils (0 to 2%), as these soils contain no The overall consumption (destruction–degradation) of clay minerals
or a very small amount of kaolinite. The proportion of smectite and/or (kaolinite, illite and smectite) is lower for the Kaol soil and I soil than for
illite destroyed is significant in the range of 8 to 17% for Sm, Sm–I, the Sm–Kaol, Sm–I and Sm soils, despite a greater amount of lime being
Sm–Kaol and I soils. available for the pozzolanic reaction (after the short-term cationic

Table 4
Analysis of results for the five lime treated clayey soils, cured at 20 °C and 50 °C.

Clay soil Kaol soil I soil Sm–Kaol soil Sm–I soil Sm soil
+ ++ ++
Proportions (%) of smectite, kaolinite and illite Smectite 0 Smectite 0 Na -smectite 48 Ca , Mg smectite 38 Ca++, Mg++ smectite 72
Kaolinite 83 Kaolinite 22 Kaolinite 38 Kaolinite 0 Kaolinite 10
Illite 10 Illite 55 Illite 0 Illite 40 Illite 15

Lime consumed (AAS) 20 °C 13–44 31–83 79–100 63–100 74–100

[in % of lime added] 1–6 months of curing 50 °C 68–100 88–100 98–100 91–100 94–100
Clay destroyed (TGA) 20 °C K: 5 K: 0 K: 20 S–I: 11 K: ≤1
ΔTG [in % of M(T0)] 6 months of curing I: 0 I: 8 S: 10 S–I: 13
50 °C K: 7 K: 2 K: 28 S–I: 14 K: ≤1
I: 0 I: 13 S: 14 S–I: 17
Ca-hydrates formed (TGA) 20 °C 2.2 1.6 3.0 1.5 2.6
ΔTG [in % of M(T0)] 6 months of curing 50 °C 3.7 2.3 3.3 3.1 3.4
144 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145
exchange) in the first two soils (9–10%) than in the last three soils (5%
to 6%). Destruction of the clay layer provides anions (SiO4)n − and
(AlOxOH6 − x)m − that are useful for Ca-hydrates formation and can
be related to the yield of Ca-hydrates. After a long maturation period
(6 months), the difference in relative mass (ΔTG) lost between 110
and 400 °C for the treated and the untreated samples is due to the
lime treatment. These mass losses are related to the amount of
water lost during the dehydration of each Ca-hydrate, and conse-
quently to the amount of Ca-hydrates formed, and can be taken as
an estimation of the relative mass of Ca-hydrates formed. The
amount of Ca-hydrates increases when the temperature increases
from 20° to 50 °C: slightly in Kaol–Sm soil, a little more in I soil and
more appreciably in the Sm, Sm–Kaol and Sm–I soils. After 6 months
at 50 °C in the treated Kaol, Sm–Kaol, Sm and Sm–I soils, the propor-
tions of Ca-hydrates are nearly equal (3.1 to 3.7%), while this is lower
in the I soil (2.3%).
4. Conclusion
The lime consumption of five clayey soils with different major clay
minerals of kaolinite, illite, smectite–kaolinite, smectite–illite and smec-
tite was studied. The kinetics of the lime treatment (10% lime) of clay
minerals and the mineralogical changes at 20 °C and 50 °C up to
6 months ageing were monitored and analysed.
Monitoring of the lime consumption explains the mechanisms in-
volved in the short-term and long-term responses of the clayey soil.
The dissolution of the lime in the water of treated soil induces an alka-
line medium (pH greater than 12), and provides OH− ions and Ca++.
It leads to cation exchange and to the partial destruction of the clay
minerals. The strength and extent of the attack depend on the crystallo-
graphic nature of the clay minerals and contribute to the formation of
bridges between the clay mineral particles, allowing their aggregation
(assembly) and inducing flocculation.
This action is induced in the early hours of treatment, changes the
appearance of the material and reduces the plastic behaviour of the
clayey soil and its sensitivity to water. The long-term reaction, induced
by the dissolved alumina and silica fractions of the clay mineral layers in
the strongly-alkaline medium is activated by the added lime in the
hydrated soil. As long as residual calcium cation is available and the
pH is high enough, the pozzolanic reaction continues. The formation
of calcium hydrates (CAH, CSH or CSAH) due to the presence of Ca++,
(OH)− and anions (SiO4)n− and (AlOxOH6 − x)m− changes the struc-
ture of the tested clayey soils at a microscopic level as shown by XRD
and TGA. The developments of Ca-hydrates are similar to those ob-
served in cementation materials, and gradually improve the mechanical
performance of the treated soils.
Monitoring of the lime consumption for these 5 treated clayey soils
shows that the entire amount of lime (10%) has been consumed after
a shorter or longer period of curing time. The kinetics of the lime treat-
ment depend on the mineralogical and crystallographic nature of the
clay mineral, on the amount of lime available, and on the curing temper-
ature. These reactions are relatively fast with smectite, slow with illite
and even slower with kaolinite. The fast cation exchange reaction im-
mediately consumes lime: 4–5% for our samples containing smectite
and nearly zero for samples with mainly kaolinite and illite.
Moreover, the results demonstrate that the pozzolanic reaction is
present and develops in all the clayey soil samples tested. This reaction
increases with the amount of lime available, and is greatly accelerated
by increasing the curing temperature from 20° to 50 °C. The slow pozzo-
lanic reaction involves lime consumption over a long period of curing
time at room temperature (20 °C). The pozzolanic reaction is practically
complete, after 6 months of curing at 20 °C, in the tested clayey soils
with a smectite component, less in illite and even lower in kaolinite.
However, all the lime is consumed in all the tested soils after 6 months
of curing at 50 °C. The faster consumption of lime by smectite can be
attributed to its CEC and to its structure (large and thin TOT layers). In
illite, the interlayer cation (K+) is very difficult to exchange, and theo-
retically kaolinite has a very low CEC (Bergaya et al., 2006), so the layers
of illite (TOT) and kaolinite (TO) are not easily opened. Therefore, the
lime available after short-term reactions is greater for kaolinite and illite
than for the smectites. Furthermore, in the Sm–Kaol soil tested,
kaolinite is highly divided and interstratified with smectite, while
in the Kaol soil, the kaolinite is well crystallised. This structural prop-
erty can also explain the greater and faster reaction of Sm–Kaol with
lime.
Whatever the mineralogical composition of the clayey soil,
treatment with lime in the presence of water induces the formation of
Ca-hydrates composed of different proportions of calcium, aluminium,
and silicon resulting from the destruction of clay minerals. CAH is
formed at 20 °C in Kaol soil, Sm–Kaol soil and I soil in the form of
Ca3Al2O6 and xH2O. At 50 °C, CAH is formed earlier and in greater
quantities in kaolinite, and later Ca3Si2O7, xH2O or Ca3Al2SiO4(OH)8
are additionally formed in smectite and Ca2Al2SiO7 and 8H2O in kaolin-
ite. Finally, the effectiveness of lime treatment in the long-term is deter-
mined by the reactivity of the pozzolanic reaction and the different
amounts of lime that are not consumed by the clay minerals in the
short-term.
Acknowledgement
The authors gratefully acknowledge the French National Research
TerDOUEST project “Sustainable earthworks involving treated soils”
funded by the French National Research Agency (ANR-07-PGCU-0006)
for providing soils (Kaol soil and Sm–I soil).
References
Al-Mukhtar, M., Lasledj, A., Alcover, J.-F., 2010a. Behaviour and mineralogy changes in
lime-treated expansive soil at 20 °C. Appl. Clay Sci. 50, 191–198.
Al-Mukhtar, M., Lasledj, A., Alcover, J.-F., 2010b. Behaviour and mineralogy changes in
lime-treated expansive soil at 50 °C. Appl. Clay Sci. 50, 199–203.
Al-Mukhtar, M., Khattab, S., Alcover, J.-F., 2012. Microstructure and geotechnical proper-
ties of lime-treated expansive clayey soil. Eng. Geol. 139–140, 17–27.
Al-Rawas, A.A., Goosen, M.F.A., 2006. Expansive Soils: Recent Advances in Characteriza-
tion and TreatmentTaylor & Francis/Balkema, London.
Arabi, M., Wild, S., 1986. Microstructural development in cured soil–lime composites. J.
Mater. Sci. 21, 497–503.
Bell, F.G., 1996. Lime stabilization of clay minerals and soils. Eng. Geol. 42 (4),
223–237.
Bergaya, F., Lagaly, G., 2006. General introduction: clays, clay minerals and clay science.
In: Bergaya, F., Theng, B.K.G., Lagaly, G. (Eds.), Developments in Clay Science 1.
Handbook of Clay Science 1, pp. 1–18 (Chapter 12.10).
Bergaya, F., Vayer, M., Lagaly, G., 2006. Cation and anion exchange. In: Bergaya, F., Theng,
B.K.G., Lagaly, G. (Eds.), Developments in Clay Science 1. Handbook of Clay Science 1,
pp. 979–1000 (Chapter 12.10).
Boardman, D.I., Glendinning, S., Rogers, C.D.F., 2001. Development of stabilisation and
solidification in lime–clay mixes. Geotechnique 51 (6), 533–543.
Diamond, S., Kinter, E.B., 1965. Mechanisms of soil–lime stabilization. Highw. Res. Rec. 92,
83–102.
Eades, J.L., Grim, R.E., 1960. Reaction of hydrated lime with pure clay minerals in soil
stabilization. Highw. Res. Board Bull. 262, 51–63.
Grim, R.E., 1962. Applied Clay MineralogyMcGraw-Hill, New York.
Hill, G.H., Davidson, D.T., 1960. Lime fixation in clay soils. Highw. Res. Board Bull. 262,
20–32.
Ingles, O.G., Metcalf, J.B., 1972. Soil Stabilization: Principles and PracticeButterworths,
Sidney.
Khattab, A.S., 2002. Comportement mécanique d'une argile gonflante stabilisée à la chaux.
(PhD Thesis) Université d'Orléans.
Khattab, S.A.A., Al-Mukhtar, M., Fleureau, J.M., 2007. Long-term characteristics of a lime
treated plastic soil. J. Mater. Civ. Eng. 19 (4), 358–366 (ASCE).
Konan, K.L., Peyratout, C., Bonnet, J.P., Smith, A., Jacquet, A., Magnoux, P., Ayrault, P., 2007.
Surface properties of kaolin and illite suspensions in concentrated calcium hydroxide
medium. J. Colloid Interface Sci. 307 (1), 101–108.
Lasledj, A., 2009. Traitement des sols argileux à la chaux: processus physico-chimique et
propriétés géotechniques. (PhD Thesis) Université d'Orléans.
Little, D.N., 1996. Fundamentals of the stabilization of soil with lime. Nat. Lime Assoc. Bull.
332, 1–20.
Liu, J., Wang, T., Yahu, Y., 2010. Experimental study of the dynamic properties of cement-
and lime-modified clay soils subjected to freeze–thaw cycles. Cold Reg. Sci. Technol.
61 (1), 29–33.
Maubec, N., 2010. Approche multi-echelle du traitement des sols à la chaux: études des
interactions avec les argiles. (PhD Thesis) Université de Nantes.
 M. Al-Mukhtar et al. / Applied Clay Science 95 (2014) 133–145 145

Rao, S.M., Shivananda, P., 2005. Role of curing temperature in progress of lime–soil
reactions. Geotech. Geol. Eng. 23 (1), 79–85.
Rojas, M.F., Cabrera, J., 2002. The effect of temperature on the hydration rate and stability
of the hydration phases of metakaolin–lime–water systems. Cem. Concr. Res. 32 (1),
133–138.
Sivapullaiah, P.V., Sridharan, A., Bhaskar Raju, K.V., 2000. Role of amount and type of clay
in the lime stabilisation of soils. Proc. ICE — Ground Improv. 4 (1), 37–45.
Stoltz, G., Cuisinier, O., Masrouri, F., 2012. Multi-scale analysis of the swelling and shrink-
age of a lime-treated expansive clayey soil. Appl. Clay Sci. 61, 44–51.
Stumm, W., 1997. Reactivity at the mineral–water interface: dissolution and inhibition.
Colloids Surf. A 120 (1–3), 143–166.
Zhou, Z.H., Gunter, W.D., 1992. The nature of the surface-charge of kaolinite. Clay Clay
Miner. 40 (3), 365–368.