Nat Hazards (2012) 61:931–942

DOI 10.1007/s11069-011-9941-2

ORIGINAL PAPER

Stabilization of tropical kaolin soil with phosphoric acid

and lime

Amin Eisazadeh • Khairul Anuar Kassim • Hadi Nur

Received: 3 September 2009 / Accepted: 10 August 2011 / Published online: 20 August 2011
Ó Springer Science+Business Media B.V. 2011

Abstract Studies on the chemically stabilized soils have shown that the effectiveness of
treatment is largely dependent on soil’s natural environment. In tropical kaolin soils,
phosphoric acid may be used as an alternative to traditional alkaline stabilizers for
improving soil properties. This research was carried out in an effort to identify the time-
dependent soil-stabilizer reactions. Data for the study of characterization of treated samples
were obtained from X-ray diffractometry, energy dispersive X-ray spectrometry, field
emission scanning electron microscopy, Fourier transform infrared spectroscopy, and
leaching analysis. Based on the collected data, the kaolinite mineral with pH-dependent
structural properties showed slightly different behavior both in basic and in acidic medi-
ums. Also, it was found that the chemical stabilizers preferentially attacked the alumina
surface of the clay particles. Therefore, it was rational to suggest that with respect to lime
and phosphoric acid treatment, aluminate hydrate compounds are more likely to be formed.

Keywords Tropical kaolin  Stabilization  Phosphoric acid  Lime 

Characterization  Leaching

1 Introduction

Natural clay minerals are well known and familiar to mankind from the earliest days of
civilization. Among these, kaolinitic clays are geochemically and industrially very ver-
satile (Manju et al. 2001). These minerals are formed under tropical weathering conditions
in areas where precipitation is relatively high, and there is good drainage to ensure leaching
of cations and iron from acidic granitic rocks (Mitchell and Soga 2005). Soft kaolin

A. Eisazadeh (&)  K. A. Kassim

Department of Geotechnic and Transportation, Faculty of Civil Engineering, Universiti Teknologi
Malaysia, 81310 UTM Skudai, Johor, Malaysia
e-mail: A.Eisazadeh@yahoo.com

H. Nur
Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia,
81310 UTM Skudai, Johor, Malaysia

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932 Nat Hazards (2012) 61:931–942

deposits are considered to have particularly poor engineering characteristics, exhibiting

expansive properties, high plasticity, poor workability, and low shear strength. Therefore,
the construction of structures on these deposits is confronted with many geotechnical
problems. In such problematic clays, chemical stabilization techniques have proven to be
effective (Ingles and Metcalf 1972).
The effect of calcium-based stabilizers on the geotechnical properties of soil has been
examined by many investigators, and rational application guidelines and laboratory testing
methods have been developed (Balasubramaniam et al. 1989; Locat et al. 1996; Bell 1996;
Narasimha Rao and Rajasekaran 1996). However, the effectiveness of technique has been
difficult to predict when applied to sulfate-rich soils (Mitchell and Dermatas 1992; Kota
et al. 1996; Rogers et al. 1996; Rollings et al. 1999).
In general, acids are effective in removing alumina and other metallic oxides from clay
minerals (Herzog and Mitchell 1963). Treatment of kaolinitic clays using phosphoric acid
has been reported to bring several beneficial changes such as improved strength and
workability (Lyons and McEwan 1962; Medina and Guida 1995). Furthermore, in addition
to being cheaper to transport than traditional bulk stabilizer materials, the nontoxic nature
of phosphoric acid is also a favorable feature, making them a potentially attractive alter-
native for treating acidic tropical soils.
The following equations can be given as the surface reactions of phosphate ion with
kaolinite (Ioannou and Dimirkou 1997):
SOH þ Hþ $ SOHþ
2 ð1Þ
 þ
SOH $ SO þ H ð2Þ
SOH þ H3 PO4 $ SH2 PO4 þ H2 O ð3Þ
 þ
SOH þ H3 PO4 $ SHPO þ H2 O þ H ð4Þ
SOH þ H3 PO4 $ SPO2
4 þ H2 O þ 2H
þ
ð5Þ
where SOH represents the surface functional group of kaolinite. Although all the exact
mechanisms have not been identified, phosphate ions are known to react with iron and alu-
minum mineral surfaces in several different ways. For instance, the phosphate anions can be
attracted to the surfaces of metallic oxides and the broken edges of kaolinite and form phos-
phorus containing compounds (Brady and Weil 1996). This is due to the fact that alumina which
is exposed at the edges of kaolinite is amphoteric and ionizes positively at low pH environment.
As a result, positive diffuse layers can develop at the edges of particles in an acid environment,
promoting positive edge to negative surface interaction (Mitchell and Soga 2005).
The primary objective of this research was to evaluate the efficacy of phosphoric acid as
a stabilizer in comparison with lime treatment and also to examine and suggest the relevant
processes responsible for the physicochemical changes induced on the structure of tropical
kaolin soils at different pH conditions.

2 Materials and experimental program

2.1 Materials

The bulk kaolin soil used in this investigation was a white, odorless, dry powder. The
physical properties of the natural soil along with its chemical composition are presented in

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Nat Hazards (2012) 61:931–942 933

Table 1 Physicochemical properties of natural kaolin soil

Engineering and physical properties Values Chemical composition (oxides) Values (%)

CEC (meq/100 g) 12.87 SiO2 48.18

pH (L/S = 2.5) 4.34 Al2O3 31.10
Specific gravity 2.66 Fe2O3 1.03
External surface area (m2/g) 19.87 MgO 0.86
Liquid limit, LL (%) 42.20 P2O5 9.37
Plastic limit, PL (%) 21.30 K2O 4.01
Plasticity index, PI (%) 20.90 SO3 2.07
IS classification CL CO2 1.34
ICL (%) 2 Soluble phosphorus (P) 5.10 ppm
Maximum dry density (Mg/m3) 1.64 Soluble aluminum (Al) 5.80 ppm
Optimum moisture content (%) 18.40 Soluble silica (SiO2) 4.00 ppm
Unconfined compressive strength (kPa) 134 Soluble calcium (Ca) 0.40 ppm

Table 1. It should be mentioned that the lime used in this investigation was a laboratory-
grade hydrated lime. In addition, the phosphoric acid was a Merck-analyzed, 85% H3PO4,
of specific gravity 1.71.

2.2 Preparation of specimens

Clause 3.3.4.1 of BS 1377: Part 4: 1990 was adopted in order to determine the optimum
moisture content of the natural soil. This moisture content was used in all mix designs, so
that the changes observed in behavior of treated samples were solely due to the stabilizer
action and not from the effects of varying water contents. Also, according to the previous
studies conducted regarding the stabilization of kaolinitic soils (Medina and Guida 1995;
Bell 1996), two different amounts of phosphoric acid and lime, i.e., 2 and 5% by weight of
the dry soil, were selected for this research. Samples were then compacted into a 50-mm-
diameter thin wall PVC tubes under constant compactive effort as specified in clause 4.1.5
of BS 1924: Part 2: 1990. They were sealed to the atmosphere with rubber tight lids and
stored in a room with constant temperature (27 ± 2°C) until being tested at 1-, 4-, and
8-month curing period.

2.3 Testing program

In this research, the stabilized soil was characterized prior to and after treatment. The
method and equipments used in each of these analyses are described as follows.
Leaching was performed based on a procedure slightly modified from the Environ-
mental society of Canada (EC 1990), known as equilibrium extraction (EE) test. This test is
based on achieving steady state conditions by stirring the treated material with distilled
water and monitoring the pH changes until it reaches a constant value (Eisazadeh 2010).
For each test, 20 g of solid particles was mixed with 160 mL of distilled water using a
magnetic stirrer for 24 h. Then, after filtration, pH was measured, and the supernatant was
preserved for ICP analysis of Si, Al, P, and Ca elements.
Powder X-ray diffraction (XRD) patterns for treated samples were measured with a
Bruker D8 advance diffractometer using CuKa radiation (k = 1.54 Å) and recording (2h)

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angles ranging from 6° to 90°. The mineralogical analysis was carried out based on the
characteristic Bragg data available in the standard Powder Diffraction File (JCPDS 1995).
The morphological features and changes in the Al/Si, Ca/Si, and P/Si ratios of treated
samples were monitored at different time intervals. Each sample was sputtered with
platinum for 120 s at 30 mA under high vacuum conditions until they were completely
coated. The samples were then examined using a JSM-6701F JEOL field emission scan-
ning electron microscope (FESEM) equipped with energy-dispersive X-ray spectrometer
(EDAX). The EDAX feature of the FESEM system allowed the detection and quantitative
analysis of the major elements present on the surface of soil particles.
Fourier transform infrared spectroscopy (FTIR) was employed in order to study the
molecular changes in the structure of treated soil. The analysis was conducted on a Perkin
Elmer Spectrum 2000 instrument using KBr pellets. Hence, the transparent KBr disks were
inserted in the instrument and analyzed with adsorption bands measured at characteristic
wave numbers between 400 and 4,000 cm-1.
Unconfined compressive strength (UCS) test was performed on cured specimens at an
axial strain rate of one percent per minute in accordance with BS 1924: Part 2: 1990. The
results were used as an index of improvement. At the end of each test, the failed soil
specimen was dried and weighed to determine its moisture content.

3 Results and discussion

The release of soluble Al, Si, P, or Ca from phosphoric acid- and lime-treated white kaolin
samples at different time intervals is shown in Fig. 1, respectively. As seen in the lime-
stabilized soil, with increasing curing time, there was a sharp reduction in the level of Ca
monitored in the aqueous solution. This was consistent with the incorporation of Ca ion
into the reaction products. On the other hand, the 5% phosphoric acid treated-samples
released a soluble P concentration of 67.5 ppm at 1-month curing period while reaching an
optimum of approximately 184 ppm after 4 months. This behavior confirmed the forma-
tion of inner-sphere complexes between the phosphate ion and the surface hydroxyl groups
at the early stages of curing. Also, due to the amphoteric nature of alumina, positive-
charged sites were developed at the edges of kaolinite minerals, thus attracting P ions to
these sites. With further curing to 4 months, an increase in the level of soluble P was
observed. This was caused by the weathering action of acid on the soil structure. It should
be noted that the reduction in the level of soluble P at longer curing periods was consistent
with the formation of new reaction products, which rendered them less soluble. According
to the soluble Al data from both plots, the acid treatment caused much higher release of Al
than the lime-treated samples while virtually reaching a constant value after 4-month
curing period. This could be explained through the time-dependent weathering action of
phosphoric acid and the higher solubility of Al ions in a low-pH environment (Brady and
Weil 1996). On the other hand, for all mix designs, little soluble Si concentrations were
observed. The reason responsible for this type of behavior was the fact that the hydroxyl
groups exposed at the surface of kaolinite particles were strongly pH sensitive. Therefore,
at high pH, there was a greater tendency for H? from the hydroxyls to go into the solution.
This tendency in turn initiated mineral dissolution directly next to a source of alumina in
the clay structure. On the other hand, at low pH, since the hydroxyl sites became positively
charged, the clay alumina was released from surface sites by protonation action. It worth
noting that a similar trend in Si, Al, and Ca release of lime-stabilized kaolin soils has been
reported by Boardman et al. (2001).

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Nat Hazards (2012) 61:931–942 935

Fig. 1 Levels of soluble Al, Si,

Si, Al and P Solution Concentration

200
182.7
P, or Ca release into the aqueous 180 184.3
solution with respect to 172.5
160
phosphoric acid and lime
treatment 140
120
100

(ppm)
78.7 WKAT5% (Al)
80 WKAT5% (Si) 73.6
67.5
60 WKAT5% (P)
40
20
0.3 0.7 0.3
0
0 2 4 6 8 10
Curing Time (Months)
Si, Al and Ca Solution Concentration

350
295.5 WKLT5% (Al)
300
WKLT5% (Si)
250 WKLT5% (Ca)

200
(ppm)

186.3
150

100
52.7
50
7.1 18.3
0.9
0 4
0.3 1.3
0 2 4 6 8 10
Curing Time (Months)

XRD graphs of natural, lime-, and phosphoric acid-treated soil are presented in Fig. 2.
As shown, kaolinite mineral was identified by its strong diffraction lines at 12.5° and 25°
2h angles (Brown 1961). The peaks observed at approximately 9° and 18° corresponded to
illite and gibbsite, respectively. Other reflections at approximately 21° and 27° implied the
presence of quartz mineral. On the other hand, for stabilized soils, all intensities of clay
mineral reflections decreased with time. This was consistent with the vigorous action of
acid on the clay structure and also the highly pozzolanic behavior of kaolinite in an
alkaline environment. Furthermore, in lime-treated samples, a new reflection attributed to
the formation of new reaction products was observed at 11.74° 2h angle. The peak was
tentatively assigned to calcium aluminate hydrate (CAH) compound (JCPDS 1995).
In this paper, EDAX was conducted in order to identify the elements present on the
surface of clay particles. Also, the intensity of peaks at various time intervals was used to
determine the relative changes induced by the chemical treatment on the soil structure.
EDAX spectra for untreated, lime-, and phosphoric acid-treated samples along with their
corresponding Al/Si, Ca/Si, and P/Si ratios are presented in Table 2 and Fig. 3a, b, c,
respectively. In the spectrum, high intensities of aluminum (Al), silicon (Si), and phos-
phorus (P) followed by lower levels of iron (Fe), magnesium (Mg), sulfur (S), and
potassium (K) were evident. Presence of these elements along with their intensity was in
good agreement with kaolinite minerals’ chemical composition (Carroll and Starkey 1971).
As shown in Table 2, there were considerable changes in the Al/Si ratio of the stabilized
samples. The increase in the Al/Si ratio of the treated samples after 4 months of curing
time is consistent with a mechanism in which compounds of aluminate hydrate gels are

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60000

50000

40000 WKAT5%8M
Lin (Counts)

30000
WKAT5%4M
20000

10000
WKAT5%1M
0
6 10 20 30 40 50 60 70 80

2-Theta - Scale

60000

50000

40000
Lin (Counts)

WKAT5%8M

30000

WKLT5%8M
20000

10000
WKUT

0
6 10 20 30 40 50 60 70 80
2-Theta - Scale

Fig. 2 X-ray diffraction patterns for untreated, lime- and phosphoric acid-treated kaolin soil at different
time intervals

Table 2 Variation of Al/Si, Ca/

Sample description Ratio (wt%)
Si, and P/Si ratios of various mix
designs with curing time Mix design Curing time (months) Al/Si Ca/Si P/Si

WKUT – 0.63 0.00 0.19

WKAT5% 1 0.77 0.00 0.52
WKLT5% 1 0.70 0.21 0.17
WKAT5% 4 0.84 0.00 0.47
WKLT5% 4 0.75 0.20 0.11
WK white kaolin, LT lime- WKAT5% 8 0.70 0.00 0.20
treated, AT acid-treated, UT WKLT5% 8 0.55 0.07 0.20
untreated

deposited on the surface of clay particles. On the other hand, after 8 months of curing, the
Al/Si ratio showed a relatively lower value. This was because of an increase in the sources
of silica present at the surface of 1:1 silica/alumina-structured kaolinite particles. This was

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Nat Hazards (2012) 61:931–942 937

also believed to be the main cause of decrease in the Ca/Si and P/Si ratios of treated
samples with curing time.
FESEM images for untreated, lime-, and phosphoric acid-treated white kaolin soil are
presented in Fig. 4a, b, c, respectively. As shown, the neatly arranged book-like kaolinite
particles are the predominant feature of the natural soil (Mitchell and Soga 2005). Com-
parison of the results indicated that the morphological changes seen in lime mix designs
were similar to those observed in phosphoric acid-treated samples but with a lesser
intensity. In addition, in both mix designs, after 8 months of curing, the formation of white
cementitious compounds on the surfaces of soil particles was apparent (Willoughby et al.
1968; Rajasekaran and Narasimha Rao 1997).
The FTIR spectra of natural and chemically treated white kaolin soil are shown in
Fig. 5. As can be seen, kaolinite was characterized by two strong bands at 3,696 and
3,620 cm-1. These bands were attributed to the octahedral OH stretching vibrations
(Madejova and Komadel 2001). In the fingerprint region, kaolinite revealed sharp bands at
1,105, 1,033, and 1,008 cm-1 attributed to the Si–O stretching and at 937 and 914 cm-1
corresponding to the OH deformation of hydroxyl groups. Most of the other bands such as
the Si–O vibrations observed at 791, 698, 540, 470, and 430 cm-1 also confirmed the
presence of kaolinite mineral. On the other hand, apparently, there were no significant
changes in the FTIR spectrums of acid- and lime-treated samples. Nevertheless, due to the
chemical attack, it seemed to be a slight decrease in the intensity of absorption band at
1,105 cm-1. Furthermore, in lime-treated samples, a new absorption band at 1,385 cm-1
attributed to the Ca–OH bond of lime was evident (Nacamoto 1970).
In order to assess the degree of improvement in the white kaolin soil, UCS test was
performed on phosphoric acid- and lime-treated samples (Ingles and Metcalf 1972).
Analysis of the data presented in Fig. 6 revealed several interesting points. First of all, the
lime mix designs obtained higher strength developments for all time intervals. Secondly,
after 8 months of curing, with respect to 5% lime and phosphoric acid treatment, an
increase of almost ten- and fivefold in the strength of stabilized soil in comparison with the
natural soil was observed. The third point worth noting was the fact that for the 2% lime-
treated samples, there was only a small gain in the strength from 4 to 8 months of curing.
Finally, considering the effects of curing time, it was also evident that with further curing,
there was a significant improvement in the strength of 5% acid- and lime-stabilized
samples. This could be explained by the slow nature of soil-chemical reactions, which were
mainly responsible for the formation of new reaction products that cemented the clay
particles together.

4 Conclusions

In this paper, the efficacy of phosphoric acid and lime treatment and moreover the
mechanisms responsible for the improvement of tropical kaolin soils were investigated.
Based on the data collected from leaching analysis, the kaolinite mineral with pH-
dependent structural properties showed slightly different behavior both in basic and in
acidic mediums. In lime treatment, negative charges were generated on the edges of clay
particles. These negative sites, which were previously involved in hydrogen bonding to
other mineral sheets, consequently attracted calcium ions in the pore water solution. On the
other hand, the protonation of soil due to inclusion of phosphoric acid and its interaction
with surface hydroxyl groups resulted in the formation of positive charges on the surface of
clay particles. In addition, the alumina sites present in the 1:1 layer-type kaolinite mineral

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006
(c) 6000
Si
5500
5000
4500 O
Al
4000
3500
Counts

3000
2500 Pt
2000 P

1500 Fe Mg Pt K Ca
Pt
C Fe SS K Ca FeKesc Fe
1000 Fe
500
0
0.00 0.80 1.60 2.40 3.20 4.00 4.80 5.60 6.40 7.20

keV
011
(b) 5500
5000 Si

4500
4000
O
3500 Al
3000
Counts

2500 Pt

2000 P
1500 Fe Mg Pt Pt K Ca
1000 C Fe S S K Ca FeKesc Fe
500
0
0.00 0.80 1.60 2.40 3.20 4.00 4.80 5.60 6.40

keV
004
4400
(a) Si
4000
3600
3200
2800 Pt
O Al
2400
Counts

2000 P
1600
1200 Fe Pt Pt
Mg SS K
800 C Fe K FeKesc Pt
Fe Fe Pt
400
0
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00

keV

Fig. 3 EDAX spectra of a untreated b lime-treated and c phosphoric acid-treated kaolin

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Nat Hazards (2012) 61:931–942 939

Fig. 4 FESEM images of a untreated, b lime-treated, and c phosphoric acid-treated kaolin after 8-month
curing period

also contributed to the development of positive charges. As a result, these positive sites
attracted phosphate ions present in the soil environment. The leaching test also revealed
further important points regarding the longer-term development of reaction products. As

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1.5

1.0
Absorbance

WKLT5%8M
0.5
WKAT5%8M

WKUT
0.0
4000 3000 2000 1000
Wavenumbers

Fig. 5 FTIR spectrum of natural kaolin and 8-month-cured phosphoric acid- and lime-treated soil

1400
Compressive Strength (kPa)

WKAT2%
1200 WKAT5%
WKLT2%
1000
WKLT5%
800

600

400

200

0
0 1 4 8
Curing Time (Months)

Fig. 6 Unconfined compressive strength (UCS) of lime- and phosphoric acid-treated kaolin soil with
different stabilizer content and curing time

was evident from the results, the chemical stabilizers preferentially attacked the alumina
surface of the clay particles. Therefore, it was rational to suggest that with respect to lime
and phosphoric acid treatment, aluminate hydrate compounds were more likely to be
formed. Also, it was found that after 8-month curing period, the phosphate and calcium
ions introduced by the stabilizers were incorporated into the reaction products, making
them less soluble in the pore water.
According to the FTIR results, the soil-stabilizer interactions at the particle level were
mainly surface-associated and that there were no fundamental changes in the molecular
structure of clay minerals.
From geotechnical point of view, the results obtained for unconfined compressive
strength test clearly indicated a considerable improvement in the engineering properties of
treated samples. In general, in comparison with acid stabilization, the lime-treated soil
gained more strength for all curing times. Also, in soil samples treated at lime contents
obtained by the initial consumption of lime (ICL) test, there was only a small gain in the
strength at longer curing periods. The latter was caused by the lack of free calcium ions
present in the soil environment to promote pozzolanic reactions.

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Nat Hazards (2012) 61:931–942 941

In conclusion, based on the data obtained from various spectroscopic and microscopic
techniques, it could be postulated that the primary ion-exchange reactions followed by a
surface alteration of the clay structure were the main mechanisms responsible for the
improvement in lime- and phosphoric acid-stabilized kaolin soil. In addition, the Ca/Si and
P/Si ratios obtained from EDAX analysis suggested that there were significant changes in
the surface composition of soil particles at different time intervals. This also emphasized
the fact that the soil-stabilizer reactions were mainly surface-associated.

Acknowledgment This research was supported by the Ministry of Higher Education (MOHE), Malaysia
under the Fundamental Research Scheme Grant Vot. 78011.

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