Nova Biotechnol Chim (2019) 18(2): 166-178 

                       DOI: 10.2478/nbec-2019-0019 
 

 

 Corresponding author: karimmoussaceb@yahoo.fr  

Nova Biotechnologica et Chimica 

Treatment and remediation by the stabilization/solidification process 

based on hydraulic binders of soil contaminated by heavy metals 

Rachid Sahnoune and Karim Moussaceb 

Laboratoire de Technologie des Matériaux et de Génie des Procédés (LTMGP), Faculté de Technologie, Université A/MIRA 

Bejaia, Route Targa-Ouzemour, Bejaia 06000, Algeria 

 
 

Article info 
 

Article history: 

Received: 21st May 2019 

Accepted: 20th November 2019 

 

Keywords: 

Contamination 

Heavy Metals 

Hydraulic Binders 

Remediation 

Soils 

Stabilization/Solidification 

 

 

 

 

 

 

 

 

 

 

 

 

Abstract 
 

Nature and the environment are affected by various human industrial and/or urban 

discharges. Remediation for this problem requires first and foremost an in-depth 

analysis and an overall characterization of the intrinsic properties of the pollution-

receiving environments. Secondly it is necessary to predict in these environments  

the behavior of dangerous chemical species (here particularly heavy metals) in the 

long term. This study focuses mainly on a detailed characterization of 4 soil samples 

sampled in vicinity of wild dump-BOULIMAT located 15 km west of the city  

of Bejaia-Algeria. The samples were characterised by atomic absorption 

spectrometry, X-ray diffraction, Fluorescence X and Infrared spectroscopy. The data 

showed high concentrations of metallic elements especially Zn (2,651.8 mg.kg-1)  

and Ni (163.44 mg.kg-1) in the soil samples. For their remediation,  

the stabilization/solidification (S/S) process with hydraulic binders appeared 

promising in reducing the polluting power of metal. This approach has considerably 

reduced the content of pollutants; 98 % removal was obtained for Ni and 99 % for Zn. 

The XRD analysis technique revealed the occurrence or absence of metallic elements 

in the crystallized phases. 
 
 University of SS. Cyril and Methodius in Trnava

Introduction 
 

For a long time, waste and landfills have posed 

a serious problem leading to various environmental 

issues that industries have created, and developing 

several diseases including respiratory, 

dermatological or other. Human is the main driver 

of technological and scientific development through 

these innovations that make life simplier and easier, 

however, he is the main author of pollution 

generation at the scale industrial (mining, steel, etc.) 

or domestic (civil) such as household waste, hospital 

waste (Stuart et al. 1998; Sefouhi et al. 2010; 

Prasadini et al. 2014). Wastes (solid, liquid, gas) 

produced are released into the environment  

in   the   form    of   landfills,    which   are    mostly  

uncontrolled, and in the presence of water, air  

and in contact with the receiving environment, 

becomes an active source of pollution developing 

complex and toxic elements with high geochemical 

mobility (Sefouhi et al. 2010), which are easy  

to transport and transfer (Prasadini et al. 2014), 

contaminating all the environment of proximity (air, 

soil, waters), thus influencing the life  

of the individual by the development of several 

diseases (cutaneous, pulmonary, neurological, etc.) 

causing an imbalance in the chain of life (Stuart  

et al. 1998; Sefouhi et al. 2010; Prasadini et al. 

2014; Belebchouche et al. 2014).  

A range of tests and experiments have been 

conducted in recent years on the analysis and 

characterization  of waste,  leaching  and  modeling  

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Nova Biotechnol Chim (2019) 18(2): 166-178 

167 

of long-term waste behavior (Bozkurt et al. 2000). 

Accordingly, this work has two objectives. The first 

is characterization of the site hosting the wild 

discharge of the region of BOULIMAT-Bejaia, 

which opens with all the types of rejections,  

by determining the physico-chemical parameters 

(pH, conductivity, moisture), amount of material  

and particle sizes (granulometry) (Qiao et al. 2007; 

Chikhi et al. 2012), composition and chemical 

speciation (XRD, FX, FTIR, TCLP, AAS) (Windt et 

al. 2007) soils that define the nature and the intrinsic 

parameters of the discharges (Planel et al. 2004; 

Laforest et al. 2007), the second objective is to study 

of the evolution of the soil stability by the addition 

of hydraulic binders (Zampori et al. 2009; Drouiche 

et al. 2019). 

The S/S method is an innovative method, which has 

been proven in the field by its treatment  

of more than 57 toxic elements (Gollmann et al. 

2010; Du et al. 2010; Moussaceb et al. 2012; 

Moussaceb et al. 2013) by: (i) chemical stabilization 

of toxic element by adsorption and/or ion exchange 

which is the consequence of the formation  

of chemical bonds between the waste  

and the hydraulic binder (Fuessle et al. 2004; 

Moussaceb et al. 2012; EPA 2014),  

(ii) solidification by the transformation of waste  

into a solid monolith for the purpose of trapping 

contaminating species inside the cementitious 

matrices (Shi et al. 2004; Moussaceb et al. 2012; 

EPA 2014) thus reducing the mobility of toxic 

chemical species (EPA 2014) that focus primarily on 

the addition of a hydraulic binder (Portland cement) 

to contaminated soil (Moussaceb et al. 2012). 

According to (Laurent et al. 2007) a study of S/S  

on samples of contaminated soil performed  

for 28 days to 1 year made the soil non-dangerous. 

Further (Rémillard 2012), reported that  

the decontamination of the soil contaminated with 

Cd, Cr, Cu, Pb, Zn (Shannon, Municipality, Canada) 

with S/S showed very good trapping results even 

after a long leaching period. Tests conducted  

by Soliditech. Inc. on a site contaminated by Pb  

and PCB in the region Morganville, New Jersey 

(USA) demonstrates a good application potential  

of the method (Bisson et al. 2012). Preliminary 

results of soil samples from the site examined in this 

work showed a high zinc and nickel content, thus 

presenting a site overload by these two elements. 

The soil samples treated by the S/S process  

for a 28-day curing period, showed retention rates  

in Zn/Ni metals of up to 99 % in the cementitious 

matrices. 

 

Experimental 
 

For an eventual physico-chemical and mechanical 

analysis of our soil samples, an arsenal  

of standardized methods (FX, XRD, FTIR, AAS)  

as well as standardized tests (granulometry, 

humidity, electrical conductivity, pH, TCLP) were 

used to achieve our objectives, namely:  

(i) determination of the intrinsic properties  

of the contaminated soil samples, (ii) improvement 

of the trapping of heavy metals inside  

the cementitious matrices (Segolene 1992). 

 
Sampling 

 

Sampling was carried out at the BOULIMAT-Bejaia 

landfill site after shovelling and evacuation  

of the first two centimeters with a stainless shovel, 

four soil samples to a depth of up to 40 cm were 

carried out according to the method of Targeted 

Sampling according to ISO 1993 and EPA 1991. 

The sampling points are shown in Fig. 1 and their 

coordinates in Table 1 (Pellet et al. 1993; Liliane  

et al. 2007; Bisson et al. 2012). 

 
Table 1. Location of soil sampling points with the decimal 

degree system (DDS). 

Sample 

Index 

Latitude (N) ° 

X 

Longitude(E) ° 

Y 

E (I) 36.789016 5.007027 

E (II) 36.789283 5.007847 

E (III) 36.789030 5.008666 

E (IV) 36.788747 5.009202 

 
Determination of selected physical parameters 

 

The soil samples were treated according to ISO 

11464, which consists of drying in the open air  

for 15 days before proceeding to physico-chemical 

analyzes (Pellet et al. 1993; Ministère du 

Développement Durable, de l’Environnement et des 

Parcs du QUEBEC 2010; Bisson et al. 2012). 

Sieving granulometry determined the particle size 

distribution of soil by fractionation on the Shakers 

SV008  sieving  machine  according to  AFNOR NF

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Nova Biotechnol Chim (2019) 18(2): 166-178 

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Fig. 1. Sampling points of the BOULIMAT-Bejaia landfill,  

the number 1-4 correspond to samplings sites of the samples 

EI-EIV (Table 1). 

 

X31-101 (Violaine 2007; Bisson et al. 2012). 

Residual moisture measurement determined the dry 

mass lost of a soil sample dried at 103±3 °C whose 

mass is constant at 40 °C, according to AFNOR NF 

X31-102 (Segolene 1992; Marie et al. 2012).  

pH (H2O) of soils was determined according to 

AFNOR X 31-103 recommends with the HANNA 

pH211 device (Segolene 1992; Liliane 2007; Kebir 

2012). Electrical conductivity was determined  

by the dissolution of a soil sample in water 

according to the solid/liquid ratio, and which is 

measured with the apparatus HANNA EC215, 

according to AFNOR NF X 31-113 (Segolene 

1992). 

                     𝑆/𝐿 =  1/5  …………… (1) 

 
Mineralogical composition – X-ray diffraction 

(XRD) 

 

X-ray   diffraction   consists   in   the   identification

of minerals by electron bombardment in the form 

of electromagnetic waves, where the atoms follow 

a specific arrangement according to the crystalline 

planes following to the BRAGG law. 

                     𝑛𝜆 =  2𝑑 ∗ 𝑆𝑖𝑛Ɵ° …………      (2) 

where 𝑛 – diffraction order, 𝜆 – X-Ray wavelength, 
d – inter-reticular distance, Ɵ° – Bragg Angle.  
The indexation of peaks allows the identification  

of mineralogical phases present by referring  

to the American Society or Testing Materials 

(ASTM) sheets. The diffractograms of our soil 

samples were obtained on the device after treatment 

with Panalatical X'pert Hight Score (Ministère du 

Développement Durable, de l’Environnement et des 

Parcs du QUEBEC 2010; Marie et al. 2012; Eti 

2012; Moussaceb et al. 2019). 

 
Fourier Transform Infra-Red (FTIR) spectrometry 

 

The FTIR is used to identify the functional groups 

existing within our soil samples following  

a vibrational transition interval between 4000 –  

400 cm-1 (Mejbri et al. 1995; Mounia 2013) with  

the spectrometer SHIMADZU IRAffinity-1S, 

samples preparation is made in KBr pellet. 

 
Chemical composition  

 

The simple extraction procedures are methods that 

run in one step, and those using several methods. 

These concluded: (i) X-ray fluorescence, which 

gives the proportions of the major elements as  

an oxide by bombardment of the sample surface with 

X photons, performed using the SKYRAY 

7000XRF experimental setup. (ii) atomic absorption 

spectrometry (Thermo Scientific ICE 3000) was 

used for the quantification of trace elements present 

in soil samples to be treated and those after acid 

leaching preparation (Toxicity Characterisation 

Leaching Procedure – TCLP) (Bisson et al. 2012; 

Drouiche et al. 2019). 

 
Leaching tests  

 

The TCLP-EPA 1311 test is a method used  

to evaluate the mobility of inorganic species in order 

to evaluate whether an industrial residue is 

considered as a dangerous leachable material or not.

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Nova Biotechnol Chim (2019) 18(2): 166-178 

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It is carried out by dissolving a soil sample 

in a solution containing 2.572 g of sodium hydroxide 

and 5.7 mL of acetic acid with a solid/liquid ratio: 

                      𝑆/𝐿 = 1/20.....................… (3) 

where the leachate recovered after filtration was 

analyzed for heavy metals by atomic absorption 

spectroscopy (AAS) (Lassin 2002; Liliane 2007; 

Moussaceb et al. 2019). 

 
Soil samples processing 

 
Once the soil samples have been characterized,  

an operation of treatment was carried out, and for 

this purpose mixtures of several variation were 

established by addition of contaminated soil 

(between 0 and 40 %) and cement. The cement used 

in this study is Portland cement CEM I from Ain El 

Kbira, Algeria. Table 2 shows the formulations 

made in accordance with standard NF P 98-230-3 

(Bozkurt et al. 2000; Prasadini et al. 2014).  

The   constituents   were   introduced   into  a  mixer 

and mixed dry for 2 min. then they spread on a non-

contaminating surface at the thickness of the largest 

grain and then the water is added by spraying  

and they are left for 28 days at a ambient temperature  

(20±3 °C) to undergo characterization tests, namely: 

XRD, FX, TCLP (Berger 2009). The realization of 

the mixtures soil/ cement is based on the report 

(Bouzeroura et al. 2018). 

                 𝑤/(𝑐 + 𝑠) = 0.5…………… (4) 

with: w – mixing water [mL], c – Portland cement 

[g], s – contaminated soil [g]. The quantities  

of cement are fixed at 450 g and those of the soil are 

varied from 0 to 40 %. The quantities used are given 

in Table 2. 

Table 2. Mixtures formulations with quantity of cement (Mc), 

water (W) and soil (S). 

Mc+S [g] Mc [g] W [mL] S [g] (s/c) ×100 [%] w/(s+c) 

495 450 247.5 45 10 0.5 

540 450 270 90 20 0.5 

585 450 292.5 135 30 0.5 

630 450 315 180 40 0.5 

 
Table 3. Granulometry parameters of soil samples (Jerome et al. 2012). 

 Laws  and Parameters Unit EI EII EIII EIV 

D5 Particles Diameter at 5 % mm 0.09 0.13 0.10 0.07 

D10 Particles Diameter at 10 % mm 0.18 0.27 0.23 0.11 

D16 Particles Diameter at 16 % mm 0.33 0.45 0.39 0.18 

D25 Particles Diameter at 25 % mm 0.61 0.76 0.67 0.34 

D30 Particles Diameter at 30 % mm 0.91 0.98 0.87 0.48 

D50 Particles Diameter at 50 % mm 1.48 1.75 1.45 1.23 

D60 Particles Diameter at 60 % mm 1.88 1.97 1.79 1.62 

D75 Particles Diameter at 75 % mm 2.52 2.5 2.45 2.32 

D84 Particles Diameter at 84 % mm 2.98 3.02 2.93 2.84 

D90 Particles Diameter at 90 % mm 3.30 3.34 3.29 3.24 

D95 Particles Diameter at 95 % mm 3.65 3.66 3.63 3.57 

Curvature coefficient 𝑪𝒄 = 𝑫𝟑𝟎
𝟐 𝑫𝟔𝟎⁄ ∗ 𝑫𝟏𝟎 C

te 2.44 1.80 1.84 1.29 

Uniformity coefficient 𝑪𝒖 = 𝑫𝟔𝟎 𝑫𝟏𝟎⁄  C
te 10.44 7.29 7.78 14.72 

Sorting index (Trask) 
𝑺𝒐 =  √

𝑫𝟕𝟓
𝑫𝟐𝟓

 
Cte 2.03 1.83 1.91 2.61 

Asymmetric Trask coefficient 
𝑺𝒌 =  

𝑫𝟐𝟓 ∗ 𝑫𝟕𝟓

𝑫𝟓𝟎
𝟐

 
Cte 0.70 0.63 0.78 0.52 

Inter-quartile 
𝜟 = √

𝑫𝟖𝟒
𝑫𝟏𝟔

⁄  
Cte 3.00 2.59 2.74 3.97 

Angularity coefficient (Kurtosis) K = 
(𝑫𝟕𝟓−𝑫𝟐𝟓)

𝟐∗(𝑫𝟗𝟎−𝑫𝟏𝟎)
 

Cte 0.30 0.29 0.29 0.31 

Porosity P = 0.13 +
0.21

(𝐷50+0.002)
0.21

 mm
-1 0.32 1.75 2.11 2.54 

Dispersion index (FOLK/WARD) D = 
(𝐷84−𝐷16)

4
+

(𝐷95+𝐷5)

6.6
 mm 1.20 1.17 1.17 1.19 

Asymmetric index of Krumbein Ski = 
(𝑫𝟕𝟓+𝑫𝟐𝟓)−(𝟐∗𝑫𝟓𝟎)

𝟐
 

mm 0.085 0.085 0.11 0.10 

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Results and Discussion  

 
Characterisation of sampled, non-treated soil  

 

Granulometry distribution was rather similar  

for tested soil samples (for EI shown in Fig. 2A) 

from values of individual parameters (Table 3) it can 

be seen that the values of the coefficients recorded 

are as follows:  curvature coefficient ranged between 

1.29 – 2.44, uniformity coefficient between 7.29 – 

14.72, sorting index (Trask) between 1.83 – 2.61, 

asymmetric Trask coefficient between 0.52 – 0.78, 

inter-quartile between 2.59 – 3.97, angularity 

coefficient (Kurtosis) between 0.29 – 0.31, porosity 

in range of 0.31 – 0.33, dispersion index 

(Folk/Ward) between 1.16 – 1.20, asymmetric index 

of Krumbein in range of 0.085 – 0.11.  

 

 
Fig. 2. Characterisation of non-treated soil samples. 

Granulometry distribution of soil sample EI and the grain 

diameters at percentage between 5 % to 95 % corresponding to 

D5 to D95 (A). Weight distribution of the same soil sample 

according to sieves series in range 0.063 – 4 mm, depending 
on the AFNOR NF X31-101 standard (B) corresponding data 

are given in Table 3. 

These data point on a varied grain size, a spread  

and poorly graded distribution, and a ranking  

of the grain size on the coarse fraction side with  

a random arrangement of poorly sorted spheres. 

(Blott and Pye 2001; Jerome et al. 2012). Thus, our 

samples represent a spreading and well graded 

particle size.  

The results in Fig. 2B show the weight distribution 

of sample EI. Highly similar pattern was observed 

for the weight distribution of EII-EIV samples  

(data not shown). It is concluded that our soil 

samples have the same weight proportions  

with a high mass presence at mean diameters  

(2 and 1.5 mm). These represent respectively  

the intervals 2 – 1 mm and d > 2mm, and which  

vary between 32.34 % – 39.57 % and 25.4 % – 32.25 

%, respectively. According to the standard  

NF P18-560 and according to the classifications  

of Strakhov and Wentworth (Jerome et al. 2012),  

it is concluded that our soil is coarse  

sand-type.  

The main properties of soil samples are shown  

in Table 4. The data show that the moisture content 

varies between 1.11 % and 3.10 %. These values are 

strongly linked to actual climatological factors 

during the moment of sampling just after  

the summer period of 2016/2017, as well as  

the presence of waste that makes the soil 

hydrophobic to water. According to Souhila (2005) 

the loss of mass in the soil does not only refer to 

water but also to the evaporation of volatile organic 

matter likely to intervene at 60 °C. The pH of soil 

samples varies between 8.05 and 8.25 (Table 4), 

suggesting that the soil is an alkaline soil (Marie 

2009), favoured by the dominant geological 

formation of the study site which is calcareous-

sedimentary formation. According to Souhila (2005) 

basic pH values have been found in the geological 

state of the studied soil and which is alkaline. 

Furthermore, Kebir (2012) reports that the basic pH 

of soil samples of the landfill refers to biological 

activity in field. 

 
Table 4. Physical parameters of soil samples according  

to AFNOR NF X31 standards. 

Sample 
Moisture  

[%] 
pH (H2O) 

Conductivity  

[mS.Cm-1]  

E I 3.05 8.20 689 

E II 2.47 8.05 1173 

E III 3.10 8.10 958 

E IV 1.11 8.25 519 

A 

B 

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Fig. 3. Infrared spectrum of soil samples from localities EI-EIV (Fig. 1) before treatment. 

The values of conductivities range from 519  

to 1,173 mS.cm-1, which is classified as slightly 

saline soil according to DURAN scale (Marie 2009). 

These values indicate a strong interaction between 

the salts present in the soil and the mineral character 

of the study site. 

Fourier transform infrared spectroscopy (FTIR) was 

applied to identify functional groups. The analysed 

soil samples have a high siliceous rock content, 

which has a vibrational domain at 2,100 cm-1  

and 1986 cm-1 and then at 1,124 cm-1 and 1162 cm-

1. For calcareous rock, there are strong transition  

at 2506 cm-1, 1,790 cm-1 and 1,400 cm-1, whereas  

the vibrational plugs of the intermolecular water 

appear at 3,408 cm-1, 3,364 cm-1, 3,396 cm-1  

and 3,378 cm-1 for samples EI, EII, EIII and EIV, 

respectively. The latter reappear at 1,637 cm-1  

and 1,634 cm-1 for EII and EIII, respectively. Similar 

results were found from an FTIR characterization 

study on soil samples from southern Brazil (Dick 

2003). Table 5 summarizes the overall results  

for each soil samples. The infrared spectrum from 

soil samples is presented in Fig. 3 and corresponding 

functional groups are characterised in Table 5. 

The results of X-ray fluorescence showed that soil 

samples EI, EII and EIII have high proportions  

of SiO2, ranging from 45.80 % to 50.37 %,  

and Al2O3 ranging from 13.77 % to 15.09 %  

(Table 6). A low CaO content of 11.67 % to 18.39 

% was recorded as well. On the other hand, the soil 

sample IV has a high proportion of CaO, which is  

of the order of 48.39 % and low levels of SiO2  

and Al2O3 (19.06 % and 7.27 %, respectively).  

The presence of metal elements in small proportions 

in the form of traces has been observed. These 

results can be explained by the fact that the soil 

samples EI, EII and EIII were taken in places with  

a high presence of silica and alumina, resulting from 

the rejections of the discharge in question, which 

consist of glasses and aluminum, and their 

provenance from the mother rock of the region 

which is rich in silicates and aluminates. On the 

other hand, the results obtained in the soil sample 

EIV are confirmed by the fact that the sampling was 

carried out on the eastern periphery of the landfill 

and close to a limestone bed (aggregate quarry).  

The metallic trace elements found in these soil 

samples   returned   to   the   nature    of   the   waste 

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Table 5. Infrared spectroscopy of the functional groups from soils samples using SHIMADZU IRAffinity-1S (Foil et al. 1952; 

Maglione et al. 1975). 

Soil Sample Wavelength 

[Cm-1] Identification Band 

EI EII EIII EIV 

ND 3626 3623 3626 Vibration Si-O-H of Clay 

3408 3363 3396 3378 Vibration OH of H2O 

ND ND ND 2506 Calcite 

ND 2108 2111 2101 Vibration Si-O of Quartz 

1986 1998 1990 2003 Vibration Si-O of Quartz 

1798 1790 1796 1796 Calcite 

ND 1637 1634 ND Vibration OH of H2O 

1407 1422 1406 1410 Calcite 

1125 ND ND 1163 Si-O of Quartz 

1035 983 1002 1009 Vibration of Si-O of Alumino-Silicate 

872 871 874 875 Vibration of CO3 of CaCO3 

ND 776 776 798 Vibration of CO3 of CaCO3 

714 ND 710 713 Vibration of CO3 of CaCO3 

ND 693 695 ND Calcite/Quartz 

663 ND ND ND ND 

607 ND ND ND ND 

517 526 522 526 Vibration of SI-O-Al 

419 447 449 465 Vibration of Si-O-Si 

discharged into the landfill (household, hospital, 

urban and industrial waste, etc.). According to 

Antonine (2012) the high abundance of CaCO3 

content refers to the presence of carbonates in rocks 

of study site and for metallic minerals in the form of 

hydroxide or sulphide. The chemical compositions 

of analysed soil samples are shown in Table 6. 

The leachates obtained by dissolving (TCLP test) 

were subjected to a chemical analysis, by AAS,  

to determine the contents of the metallic elements.  

It is found that the contents of the soil samples 

(Table 6) perfectly meet the AFNOR NF U44-041 

(1985) (Segolene 1992) standard except for [Ni] >  

50 mg.kg-1 in the soil sample EI and [Zn] >  

300 mg.kg-1 in the soil sample EIII. The results 

shown in Table 6 can be justified by acid rain, which 

frequently affects the region, thus promoting  

the migration of heavy metals through leachates that 

percolate from the landfill to the surrounding soil. 

According to Kebir (2012) the persistence of these 

metallic elements concentrations refers to the origin 

of the waste as well as to the industrial effluents 

discharged into the landfill. 

According to the XRD results, the soil has  

a similarity in initial mineralogical composition, 

which is a clay soil consisting mainly of quartz  

and calcite, with heterogeneity in the secondary 

phases that show contamination with heavy metals.

Examples include Dwornikite and Retgersite for EI 

and Wurtzite, Hopeite and Hetaerolite for EIII.  

The diffractograms of soil samples EI and EIII are 

shown in Fig. 4, while the corresponding 

mineralogical phases are summarized in Table 7. 

Table 6. Chemical composition of the analysed soil samples 

from localities E-EIV. 

                     Soil sample 

  EI  EII  EIII  EIV 

Compound content  [%]a 

SiO2 50.37 47.07 45.80 19.6 
Al2O3 15.9 13.77 14.9 7.27 

Fe2O3 4.74 5.2 5.14 4.17 

CaO 11.67 16.20 18.39 48.39 
MgO <0.05 ND ND 0.79 

Na2O <0.05 <0.05 <0.05 <0.05 

K2O 2.7 2.2 2.4 1.7 

TiO2 0.48 0.46 0.48 0.23 

MnO 0.09 0.20 0.13 0.19 

P2O5 0.28 0.42 0.35 0.76 

SO3 0.09 0.15 0.05 0.021 

NiO 0.0028 0.0035 0.0026 <0.005 

ZnO 0.0088 0.0071 0.0056 0.019 
PbO 0.0031 0.0028 0.0057 0.0123 

Metal content [mg.kg-1]b 

Zn  9.388 4.194 2651.8 20.78 

Ni   163.44 38.3 0.22 <Ld 

Pb  0.4 <Ld 3.4 2 
a Data obtained by X-ray fluorescence. 
b According to AFNOR NF U44-041 standard, after TCLP 

leaching test.

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Table 7. Mineralogical Composition of EI Sample using X’pert High Score. 

Mineral phases Chemical composition References pattern 

Soil sample EI   

Quartz SiO2 01-078-1252 

Calcite CaCO3 01-083-1762 

Urea CO(NH2)2 01-086-2276 

Muscovite KAl3Si3O10(OH)2 01-075-0948 

Despujolsite Ca3Mn(SO4)2(OH)6(H2O)3 01-072-0388 

Tridymite SiO2 01-075-1323 

Dwornikite (Ni, Fe)SO4.H2O 00-035-0558 

Argentopyrite AgFe2S3 00-038-0459 

Domeykite Cu3As 00-044-1475 

Manganotapiolite (Mn, Fe)Ta2 00-049-1870 

Retgersite NiSO4(H2O)6 01-075-0937 

Kyanite Al2SiO5 01-076-0170 

Hatrurite Ca3SiO5 01-086-0402 

Soil sample EIII   

Hetaerolite  Mn2O4Zn 00-024-1133 

Rostite  Al(SO4)(OH).5H2O 00-041-1382 

Quartz  SiO2 01-078-1252 

Calcite  CaCO3 01-083-0578 

Hopeite  Zn3(PO4)2.4H2O 00-001-0975 

Halloysite  Al2Si2O5(OH)4 00-003-0184 

Sarcopside  Fe3(PO4)2 00-039-0341 

Anthophyllite  Mg7(Si8O22(OH)2) 01-075-0909 

Collinsite  Ca2Mg(PO4)2.2H2O 00-026-1063 

Clinzoisite  Ca2Al3(SiO4) (Si2O7)(O, OH)2 00-021-0128 

Chalcocite  Cu2S 00-023-0961 

Wurtzite  ZnS 01-072-0162 

Reinhardraunsite Ca5(SiO4)2(OH)2 00-029-0380 

Linthian Saponite Na0,2(Mg,Li)3Si4O10(OH)2.4H2O 00-025-1385 

Quartz SiO2 01-078-1252 

Calcite CaCO3 01-083-1762 

Urea CO(NH2)2 01-086-2276 

Muscovite KAl3Si3O10(OH)2 01-075-0948 

Despujolsite Ca3Mn(SO4)2(OH)6(H2O)3 01-072-0388 

Tridymite SiO2 01-075-1323 

Dwornikite (Ni, Fe)SO4.H2O 00-035-0558 

Argentopyrite AgFe2S3 00-038-0459 

Domeykite Cu3As 00-044-1475 

Manganotapiolite (Mn, Fe)Ta2 00-049-1870 

Retgersite NiSO4(H2O)6 01-075-0937 

Kyanite Al2SiO5 01-076-0170 

Hatrurite Ca3SiO5 01-086-0402 

It is concluded that physico-chemical characteri-

zation study of the project site samples, which all  

the results obtained; converge towards the same 

conclusion suggest contamination of the site by zinc 

and nickel, posing a great danger to the environment, 

fauna and flora as well as to human health. 

 
Characterization of S/S soil samples 

 

Decontamination of the contaminated sites is impe- 

rative, therefore a soil process has been proposed, 

namely remediation by S/S process with hydraulic 

binders. After such treatment, FTIR analysis 

revealed the disappearance of several vibrational 

bungs and the appearance of others such as ettringite 

at 3,400 cm-1 and C-S-H at 1,400 cm-1 and 1,000 cm-

1 (Fig. 5). Further, the bung of calcite was detected. 

Similar results were found in a study reported  

by Catherine (2003). The functional groups 

corresponding to data in Fig. 5 are given in Table 8. 

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174 

20 30 40 50 60 70

0

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1213

10

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4

C
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  t
  s

   
o

  f
   

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  I

   
[ 

 %
   

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2 T h é t a [  ° ]

A

 

20 30 40 50 60 70

0

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96

14

3
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129713

34
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43

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E
  
I 

 I
  
I 

  
[ 

 %
  
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    2  T h é t a  [ ° ]

B

 

Fig. 4. X-ray diffraction of non-treated soil samples EI (A) and 

EIII (B) after treatment with Panalatical X'pert Hight Score. 

4000 3500 3000 2500 2000 1500 1000 500
40

50

60

70

80

90

100

2102,45

3398,17

448,32

516,97

713,76

870,9

1003,62

T
 r

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 I

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 /

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 /
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  [
  %

  ]

W a v e l e n g t h  [ C m 
-1

 ]

1401,79

A

 

4000 3500 3000 2500 2000 1500 1000 500 0

50

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463,14

518,43

713,14

873,39

1000
1410,25

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T
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  I
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  S
  /

  S
   

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  5

  0
  /

  1
  8

  0
   

[ 
%

  ]

W a v e l e n g t h  [ C m 
-1

 ]

3400

B

 
Fig. 5. Infrared spectra of the stabilized / solidified soil sample 

EIS/S450/180 (A) and EIIIS/S450/180 (B).  

10 20 30 40 50 60 70

0

2000

4000

6000

8000

10000

172
4

85

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86
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S
  
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 4

  
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2 T h e t a [ ° ]

A

20 30 40 50 60 70

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14

15

9

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1131

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46

26

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C
  
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5
  
0
  
/ 

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%

  
]

2  T h e t a [  ° ]

B

 

Fig. 6. X-ray diffraction of soil samples EIS/S (450/180) (A) 

and EIIIS/S (450/180) (B) after treatment with Panalatical 

X'pert Hight Score. 

Table 8. Infrared spectroscopy of the functional groups from 

Stabilized/Solidified samples soils using SHIMADZU 

IRAffinity-1S. 

Wavelengths for each Samples  

(Cm-1) 

EIS/S EIIIS/S Identification Band 

3398 3400 Hydrated Ettringite  

2103 2120 Vibration OH (H2O) 

1402 1410 C.S.H 

1004 1000 C.S.H 

871 873 Ettringite 

714 713 Vibration of CO3 (CaCO3) 

517 518 Gibbsite 

448 463 Gibbsite/Silicate 

The X-ray fluorescence results obtained on the EI 

and EIII samples of the S/S soil are recorded  

in Fig. 6 and Table 9. The results obtained show that 

CaO content in soil samples EI and EIII decreased 

due to remediation process from 11.67 %  

and 18.39 % (before S/S) to 46.08 % and 55.84 % 

(respectively), due to the accumulation of CaO 

proportions present in the soil and the cement after 

the hydration phenomenon On the other hand,  

content of both SiO2 and Al2O3 decreased after S/S;

A 

B 

A 

B 

A 

B 

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Table 9. Chemical composition from soil sample EIS/S450/180 in oxidation form by the X-ray fluorescence. 

Sample (ES/S) 
EIS/S EIIIS/S 

450/0 450/45 450/90 450/135 450/180 450/0 450/45 450/90 450/135 450/180 

Cement/Soila           

SiO2 14.62 12.82 17.47 17.83 16,82 14.62 15.26 16.55 19.41 21.23 

Al2O3 2.4 3.9 2.62 2.76 2.5 2.4 2.6 2.5 2.9 3.49 

Fe2O3 2.31 3.9 2.86 2.94 2.71 2.31 2.58 2.74 2.97 3.26 

CaO 53.00 46.08 48.13 48.26 51.35 53.00 51.86 49.49 48.86 46.06 

MgO 1.36 1.55 1.5 1.65 1.7 1.36 1.25 1.38 1.58 <LD 

K2O 0.52 0.67 0.58 0.59 0.58 0.52 0.55 0.56 0.67 0.77 

TiO2 0.20 0.37 0.27 0.31 0.25 0.20 0.23 0.25 0.3 0.34 

MnO 0.04 0.04 0.048 0.044 0.041 0.04 0.05 0.05 0.05 0.06 

P2O5 1.5 0.98 0.95 1.6 1.4 1.5 1.3 0.93 0.98 0.82 

SO3 <LD 0.12 0.014 0.007 <LD <LD <LD <LD <LD 0.17 

NiO <LD <LD <LD <LD <LD <LD <LD <LD <LD <LD 

ZnO <LD <LD <LD <LD <LD <LD <LD <LD <LD <LD 

PbO <LD <LD <LD <LD <LD <LD <LD <LD <LD <LD 

Metal contentb           

Ni [mg.kg-1] nd 0.17 0.32 0.42 1.69 nd nd nd nd nd 

Retentions rate [%] nd 97.68 97.82 98.09 94.25 nd nd nd nd nd 

Zn [mg.kg-1] nd nd nd nd nd nd 0.21 9.1 23.73 30.70 

Retentions rate [%] nd nd nd nd nd nd 99.82 96.22 93.37 93.56 
a Data obtained by X-ray fluorescence. 
b According to AFNOR NF U44-041 standard, after TCLP leaching. 

the SiO2 content dropped from 50.37 % and 45.80 % 

of the two samples to 12.82 % and 15.26 % after S/S, 

respectively. This decrease results from incorpo-

ration of SiO2 from Quartz.  As for Al2O3 the values 

of 15.09 % and 14.09 % of non-treated EI and EIII 

soil samples decrease to 3.09 % and 2.06 % after 

S/S, respectively. This decrease is due to growth  

of hydration phases of cement and more specifically 

C.S.H and ettringite for Al2O3. 

The presence of SO3 in our S/S materials refers  

to the formation of the cement phase (ettringite) 

 as well as the presence of sulphur in the soil  

and cement. The variation of the values of Si, Al, S 

and Ca refer to the hydration reaction between  

the materials of soil and those of hydraulic binder; 

they are mobilised to form hydrates of cements after 

S/S (Saussaye et al. 2016). On the other hand,  

the absence of the metallic oxides in the samples 

before S/S can be explained by the mechanism  

of substitution of elements with those of cement  

and which made it possible to trap chemically  

and physically the metallic elements inside cement 

matrix. S/S of soil samples resulted in strong 

retention of the contents of Ni and Zn; their content 

increased to 98.09 % for (Ni) and 99.82 % for (Zn) 

in the soil samples EIII and EI, respectively 

(Table 9). 

X-Ray diffraction results obtained on S/S treated 

sample EI (450/180) and EIII (450/180) are given  

in Fig. 6. The soil sample EI exerted disappearance 

of certain mineralogical phases such as retgersite  

(NiSO4 (H2O)6), but the appearance of other 

mineralogical phases such as sodium nickel sulfite 

hydroxide hydrate (NaNi (SO3)2 OH H2O). For soil 

sample EIII the disappearance of certain mineralo-

gical phases such as hopeite (Zn3 (PO4)2 4H2O)  

and the appearance of other phases, such as 

descloizite (Pb (Zn, Cu) VO4 (OH)) was observed  

in (Table 10). 

Compared with the work of Berger (2009)  

on substitutions of metallic trace elements with  

the phases of cement (natural or synthetic, total  

or partial) we found that for the two phases found 

after S/S, there is a probability of substitution of (Ni) 

from sodium nickel sulfite hydroxide hydrate with 

(Al) of ettringite for sample EI, and (Pb, Zn) from 

descloizite with (Ca) of ettringite for Sample EIII 

(Table 11). 

 

Conclusion  
 

This study analyzed the influence of the addition of 

hydraulic binder to the contaminated soil as well as 

of the proportional addition from cement trapping of 

heavy metals in cementitious matrices. Our results 

showed  that   granulometric  characteristic   of  soil 

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Table 10. Mineralogical composition of soil samples EIS/S (450/180) and EIIIS/S (450/180) using X’pert High Score. 

Mineral phase Chemical composition Reference pattern 

Soil sample EI 

Sophiite Zn2(SeO3)Cl2 00-045-1463 

Galaxite MnAl2O4 00-001-1302 

Fayalite Fe2SiO4 01-071-1669 

Ferrocarpholite (Fe0, 76 Mg0, 24)2Al4(Si4O12) (OH) 8 01-081-1503 

Nickelbischofite NiCl2.6H2O 00-025-1044 

Ettringite Ca6Al2(SO4)3 (OH)12.25H2O 00-009-0414 

Ammonium nickel chromium oxide hydrate (NH4)2Ni(CrO4)2.6H2O 00-021-0705 

Nickelboussingaultite (NH4)2Ni(SO4)2.6H2O 00-031-0062 

Nickel sulfite hydrate NiSO3.2H2O 00-034-0315 

Potassium nickel selenate hydrate K2Ni(SeO4)2.6H2O 00-035-0774 

Sodium nickel sulfite hydroxide hydrate NaNi2OH(SO3)2.H2O 00-037-0016 

Fersilicite FeSi 00-038-1397 

Nickel trans-[dichlorobis(2-oxopropyl-

diphenylphosphine)]  
C30H30Cl2NiO2P2 00-040-1756 

Brucite Mg(OH)2 01-082-2455 

Clinohedrite CaZn(SiO4) (H2O) 01-083-2269 

Bementite Mn6, 927(Si6O15) (OH) 8 01-082-1236 

Cummingtonite Mg7Si8O22(OH)2 01-072-0114 

Soil sample EIII 

Calcite CaCO3 01-083-0578 

Tachyhydrite CaMg2Cl6.12H2O 00-034-0788 

Burbankite (Na2Ca)(Sr2Ca)(CO3)5 00-026-1374 

Anilite Cu7S4 00-024-0058 

Descloizite Pb(Zn, Cu)VO4(OH) 00-041-1369 

Reinhardbraunsite Ca5(SiO4)2((OH)F) 01-075-1709 

Tobermorite (CaO)x SiO2 zH2O 00-006-0005 

Brushite CaPO3(OH).2H2O 00-009-0077 

Zinc malonate dihydrate C3H2O4Zn.2H2O 00-024-1990 

Zinc selenate hydrate ZnSeO4.H2O 00-026-0004 

Pyrophyllite Al2Si4O10(OH)2 01-074-1037 

Quartz SiO2 01-083-2473 

Ettringite Ca6Al2 (SO4)3(OH)12·26H2O 00-041-1451 

Palmierite K2Pb(SO4)2 00-020-0902 

Calcium zinc aluminium oxide Ca3Al4ZnO10 00-049-0280 

Muscovite KAl3Si3O10(OH)2 01-071-1049 

 
Table 11. Mineralogical composition from the probability of substitution phases in selected soil samples. 

Phase type Chemical formula 

Soil Sample EI S/S (450/180)  

Sodium nickel sulfite hydroxyde hydrate (Na Ni2 OH (SO3)2 H2O) 

Clinohedrite (CaZn)(SiO4)(H2O) 

Soil Sample EIIIS/S (450/180)  

Descloizite (Pb (Zn, Cu) VO4 (OH)) 

Calcium zinc aluminium oxide (Ca3 Al4 Zn O10) 

 
samples increased because the mineral composition 

of the limestone rocks dominates on the site, alkaline 

pH which defines the nature of the sedimentary 

rocks, and causes very high soil conductivities.  

We identified the profiles of present major elements 

as well as metallic elements in the mineralogical 

structure of soil samples. The high concentration  

of Ni and Zn detected in the soil surrounding  

the landfill probably results from leaching with acid 

rain that caused a migration of trace metallic 

elements from waste to soil. 

The analyses and characterizations of our S/S 

samples revealed new functional groups belonging 

to cement phases such as ettringite and C.S.H. 

Further, X-ray Fluorescence results suggest that  

the metallic trace elements disappear from soils 

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177 

because they are likely trapped inside  

the cementitious matrices. Elevated proportion  

of CaO and decreased contents of SiO2 and Al2O3  

in the soil samples might results from cement 

interaction with the soil during its hydration. AAS 

confirmed Ni and Zn retention rates of up to 98 %. 

X-ray Diffraction analyses revealed disappearance 

of certain mineralogical phases with metallic trace 

elements after the treatment. On the other hand, 

hydrated cement phases were identified, such as 

ettringite, portlandite and C.S.H in the form  

of tobermorite with presence of metallic trace 

elements. Substitution occurred between  

the metallic trace elements and the elements  

of the hydrated cement. It is concluded that the S/S 

process using hydraulic binders represents  

a promising method in the treatment  

of contaminated soils. 

 

Conflict of Interest 
 
The authors declare that they have no conflict of interest. 

 

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