IACSIT International Journal of Engineering and Technology, Vol. 5, No.

1, February 2013

Physico-Chemical Characterization of Limestones and

Sandstones in a Complex Geological Context, Example
North-East Constantine: Preliminary Results
Benyamina Mounia, Bouchear Merzoug, Benabbas Chaouki, and Ait Abdelouahab Djaouza


gray limestone, and sandstone have been collected
Abstract—The geological context of North East Constantine respectively at Jebel Kellal (mainly carbonated chain link
is very complex. This region is characterized by a superposition Cenomanian-Turonian age and east-west direction) and at the
of several thrust sheets, reflecting a geological and tectonic
evolution during Mesozoic and cenozoic.
southern massif of Jebel el Ouahch, their geographical
In addition, there is a wide variety of sedimentary rocks, such positions are given in Table I.
as limestones, sandstones, clays and marls. A physico-chemical
TABLE I: POSITIONS OF GPS SAMPLES
characterization of the lithological diversity would be a great
contribution to the different users and managers at a time when Latitude Longitude
the region is under major socio-economic development projects.
White limestone 36 °25 '27'' 6 °38' 46''
This study proposes a first phase, a physico-chemical
characterization of limestones and sandstones (by optical Gray limestone 36 °25 '25'' 6 °38' 45''
microscopy, XRD, SEM/EDS and porosimetry), and a reflection Sandstone 36 °23 '40'' 6 °39' 59''
on the development of mechanical properties of these materials
in a second phase. Rocks and sliced sugar using a chainsaw are glued to a
Preliminary results of this multidisciplinary study (obtained glass slide, reduced by a grinder in thin film which is
by various analytical techniques) show good agreement on the
polished to a thickness micrometer will be used for optic
existing phases.
observation (Laboratory of Geology and Environment, LGE,
Index Terms—Limestone, porosity, sandstone, SEM /EDS. Constantine University 1, Algeria).
The same rocks are crushed, and sieved to a particle size ≤
80 [µm]. This powder will be used for X-ray diffraction
I. INTRODUCTION analysis (XRD) and scanning electron microscope (SEM)
There is an abundance of sandstone and carbonate equipped by EDS analysis system.
formations in Constantine's region. Limestone and sandstone The micrographs taken by polarizing microscope of
taken from the north-east of Constantine is distinguished by prepared thin sections are observed in natural light using an
several features. optical microscope (Leitz brand).
The establishment and evolution of these rocks took place The XRD analysis was performed by a diffractometer
in a complex geological context marked by changed model PANalytical (Birine Nuclear Center, Ain Ouassera)
paleogeographics, paleoclimatics and pd aleotectonics. with Cu anode, λCU = 1.5406 [A°], on uncompressed powders
These changes have influenced the quality and performance in order to collect the maximum of the diffraction lines and a
of these materials. better identification of the phases.
The use of these rocks in development projects, in
The pellets are prepared from powders of particle size ≤ 80
particular in the construction of roads and highways
[µm] using a hydraulic press at a pressure of 75 [mPas] for 60
(embankments, layer shapes, art works.....), requires a better
[s], and then dried in open air, for the environmental SEM
knowledge and a thorough study of the physico-chemical
analysis (ESEM), Quanta 200 model, equipped with a
characteristics properties of these rocks in the rough.
micro-energy dispersive analysis (EDS) (Quan Tax QX2,
ROENTEC), (Process Engineering Laboratory, University of
Bejaia, Algeria).
II. EXPERIMENTAL PART
B. Optical Microscopy
A. Extraction and Preparation of Samples (Methodology)
The optical micrographs of white limestone are shown in
The elaboration samples in this study: white limestone, Fig. 1 and Fig. 2, and those of gray limestone, in Figs. 3, 4
and 5, and finally Numidian sandstones are shown in Fig. 6.
Manuscript received October 20, 2012; revised November 20, 2012.
Benyamina Mounia and Bouchear Merzoug are with the Materials The white limestone (Fig. 1) are formed by organism's
Sciences and Applications Research Unit , Department of Physics, Faculty of debris, have worn bivalve shell which are perforated by
Exact Sciences, University of Constantine 1, Algeria (e-mail:
bacteria on a background of CaCO3 carbonates and
[Link]@[Link]; m_bouchear@[Link]).
Benabbas Chaouki and Ait Abdelouahab Djaouza are with the Geology CaMg(CO3)2 dolomite. The bivalves fragment are to be in
and Environment Laboratory, Department of Earth Sciences, Faculty of micritic matrix (carbonated mud about 1 to 4µm), formed by
Earth Sciences, of geology and Planning, University of Constantine 1,
Algeria (e-mail: lgementouri@[Link]; djaouza@[Link]).
CaCO3 and dolomite CaMg(CO3)2.

DOI: 10.7763/IJET.2013.V5.523 114

 IACSIT International Journal of Engineering and Technology, Vol. 5, No. 1, February 2013

Fig. 1. Thin-section photomicrograph of white limestone, natural light. Fig. 4. Thin-section photomicrograph of gray limestone, natural light.

Fig. 2. Thin-section photomicrograph of white limestone, natural light. Fig. 5. Thin-section photomicrograph of gray limestone, natural light.

Fig. 3. Thin-section photomicrograph of gray limestone, natural light.

Fig. 6. Thin-section photomicrograph of sandstone, natural light.
The Fig. 2 shows a finer organism debris and the
fracturation porosity with calcitic filling (Fig. 2), [1]-[4]. C. X-Ray Diffraction
The gray limestones (Fig. 3) are richer in organism debris, X-ray diffraction spectra of the three types of rocks: white
essentielly formed by bivalve fragments, a rare fragments of limestone (CB), gray limestones (CG) and the Numidian
echinoderms and micritic microbreccias. the porosity type is sandstone (GN) are shown in Figs. 7-9 respectively.
vacuolar [10]-[11], the fracturation is very abundant in this The X ray diffraction pattern of sample CB1 and CG2 are
facies and shows cimenting by calcite or iron oxides (Fig. 4), presented in Figs. 7, 8: The Dolomite's pics are clearly appear
[1]. Show a significant amount of bivalve shell (marine (according to ASTM) on the pattern, they are not indexed,
fossils) and echinoderm, respectively (Fig. 3 and Fig. 4). whilst the calcite pics and Aluminium ones with the
The Fig. 5 shows a void filled with zoned calcite, so the Dolomite are indexed on the pattern.
calcite can be zoned (Fig. 5), [1]. One can note from the 3 spectrums:
Sandstone, (Fig. 6) has quartz as a main phase with size For X-ray diffraction presented in Fig. 7, one can see
grain varies from about 50 to 400 [µm] and can reach average presence of 2 important phases in the white limestone: the
600µm, with oxides and clays as phyllosilicates in CaCO3 carbonate and CaMg(CO3)2 dolomite, the minor
intergranular contacts, [2]-[3]-[11]. elements are showing by the peaks of lower intensities.

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For X-ray diffraction of Fig. 8, the gray limestones exhibit D. Analysis by Scanning Electron Microscopy SEM / EDS
the same phases exist in the white ones, but there's a The observation of the morphology using the scanning
difference in their respective amounts, with other minor electron microscope of the white limestone, gray and
elements. Numidian sandstone is reported in Figs. 10-12 respectively.
The X-ray diffraction of Fig. 9, shows that the The three observed morphologies show that:
predominant phase is quartz, calcite, minor elements: Mg2C3 One can observed from the SEM morphology of white
and Al203. limestone (Fig. 10), that's the predominant phase in the
carbonates with pores filled with organic fragments (fossil's
fragment) and an open -porosity in some areas, [5].
For the gray limestones (Fig. 11), they have a more
compact morphology, so the gray limestones have less
porous then white one and the carbonates represent the main
phase with calcite peaks [6].
For the Sandstones (Fig. 12), they have a morphology with
angular grains of quartz size around:10 to 30 [µm] , covered
with fine particles and the grains of calcite appear clearly.
This analysis of the morphology by SEM is associated by
EDS analysis of the elements exist on choised line on area
with maximum amount of informations as it is showing in:
Fig. 13 and Table II, Fig. 14 and Table III, Fig. 15 and Table
IV, respectively, for white limestone, gray limestone and
numidian sandstone.
For white limestone (Fig. 13), the presence of Ca, O, C,
Fig. 7. XRD spectrum of white limestone. Mg as major element confirms the importance of carbonate
phases, CaCO3 and CaMg(CO3)2, same remarks have been
observed in gray limestones (Fig. 14), except, that the amount
of carbonates are not the same.
The sandstones (Fig. 15) have a very important percentage
of Si and O, with the oxides and the intergranular
phyllosilicates such as: the Montmorillonite (Na, Ca)0,3(Al,
Mg)2Si4O10 or the
Kaolinite (Al2Si2O5) as minor elements observed by
optical microscopy.

Fig. 8. XRD spectrum of grey limestone.

Fig. 10. SEM morphology of white limestone (X 1600)

Fig. 9. XRD spectrum of numidian sandstone. Fig. 11. SEM morphology of gray limestone (X 1600)

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TABLE III: ELEMENTAL ANALYSIS OF GRAY LIMESTONE.

Element Wt % At %
CK 17.85 29.09

OK 41.72 51.05
MgK 00.22 00.18

AlK 00.09 00.06

SiK 00.12 00.08
CaK 40.01 19.54

Fig. 12. SEM morphology of sandstone (X 1600)

Tables: Table II, Table III and Table IV represent the

percentage of important elements and minor elements that
represent the oxides and the intergranular phyllosilicates
observed by optical microscopy.

Fig. 15. Energy dispersive microanalysis EDS numidian sandstone.

TABLE IV: ELEMENTAL ANALYSIS OF NUMIDIAN SANDSTONE.

Element Wt % At %
CK 05.12 08.63
OK 45.05 57.02
NaK 00.08 00.07
MgK 00.22 00.18
AlK 02.37 01.78
Fig. 13. Energy dispersive microanalysis EDS on the white limestone.
SiK 41.18 29.69
TABLE II: ELEMENTAL ANALYSIS OF WHITE LIMESTONE. KK 00.50 00.26
CaK 02.50 01.26
Element Wt % At %
TiK 00.41 00.17
CK 17.47 26.78
FeK 02.57 00.93
OK 46.15 53.10
MgK 10.71 08.11 E. Porosimetry
AlK 00.37 00.25 The void ratio N (%) is calculated by hydrostatic weighing
SiK 00.75 00.49 method that is based on the Archimeds methode, [7]-[9] and
KK 00.30 00.14 immersed in distilled water.
CaK 24.25 11.14
This method is applied on the three types of rocks and
obtained a good approach of porosity ratio (N). The test is
repeated 3 times on two samples for each rock.
The empirical formula [7]-[8], Refer to ''(1)'' , is applied for
the calcul of the rate's porosity [%], measures are reported in
Table 5.

N = [(Msat - Ms)/ (Msat - Mhyd)]  100 (1)

with: Ms = Mass of the dry rock.

Msat = Saturated mass.
Mhyd = Hydrostatic mass.
It is clear that the white limestones are more porous than
the gray limestones, due essentially to the difference in
texture (grain size) and the phenomena of dissolution and
erosion, this does not prevent the growth of fossil and calcite
Fig. 14. Energy Dispersive Microanalysis EDS gray limestone in the pores or grains.

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TABLE V: RATE OF POROSITY.

white limestone gray limestone Numidian sandstone
Samples 1 2 1 2 1 2
Ms [gr] 28.8155 43.6143 23.9864 30.5848 19.1125 28.6278
Msat [gr] 29.4927 44.6714 24.2194 30.8764 19.4035 29.0271
Mhyd [gr] 17.3188 26.4816 15.1377 19.5013 11.4157 17.2556
N% 5.5627 5.8114 2.5655 2.5634 3.6430 3.3920
Nmoy% 5.6870 2.5644 3.5175
TVacuum[h] 1 1 1 1 1 1
T imbibition[h] 48 48 48 48 48 48

The sandstones represent a midium degree of porosity, [4] C. Volery, E. Davaud, C. Durlet, B. Clavel, J. Charollais, and B. Caline,
Sedimentary Geologie, vol. 230, no. 1-2, pp. 21-34, 2010.
because on one hand the size of the quartz grains is important [5] Information. pp. 193-205. [Online]. Available: [Link]
and in the other hand, the intergranular voids are filled with ULgetd-02012010-134403/unrestricted/these
oxide and phyllosilicates. [6] K. Besnard, “Evolution physico-chimique des matériaux carbonatés en
milieux triphasique,” pp. 14, 2000.
[7] K. Beck, “Etude des propriétés hydriques et des mécanismes
d'altération de pierres calcaire àforte porosité,” pp. 72-75, 2006.
III. CONCLUSION [8] P. Bérest and Co, Manuel de mécanique des roches, tome1, Ecole des
mines, Paris, 2000.
The obtained results by different analyses: optical, XRD, [9] K. E. Yank, “Caractérisation du comportement mécanique des bétons
SEM / EDS and porosimetry, are in a good agreement and de granulats légers: Expérience et modélisation,” pp. 72-74, 2008.
confirm the highlight of existing of the phases in our samples. [10] J. Elsen, Cement and Concrete Research, vol. 36, no. 8, pp. 1416-1424,
2006.
The phases observed by optical microscopy of three [11] Rock and GEM, 2th ed, DK and Smithsonian, by Ronald Louis
samples are found by X-ray diffraction, the SEM Bonewitz, pp. 54-65, 2008.
morphology coupled with EDS analysis shows what has been
observed by previous techniques, confirms the existence of
element's proportions.
A reasonable degree of porosity in the limestones confirm Mounia Benyamina obtained: B.S. Material Physics,
the work done by Katia BESNARD [6], it Constantine University, Algeria in 1983, M.S. Physics
is mainly due to the difference in the texture of the (On resistance of concrete to aggressive solutions ),
specimens. Constantine University, Algeria in 1994, Ph.D. Physics
One note that the degree of porosity in the gray limestone (work is underway ) on the physico-chemical
characterization of local raw materials and their
is lower than that of white limestone, which is observed applications. She worked as assistant-lecturer, then
before in the optical micrographs where the compactness in Course Instructor from 1983-2012, She has taught for
gray limestone is higher than that in whites, so more porous. 30 years, general physics and biophysics at the department of physics and
These preliminary analyses will be followed by the study biology at Constantine university in Algeria. Currently she is working on the
physico-chemical characterization of local raw materials and their
of : applications through collaboration between laboratories for the development
The effect of temperature on the physico-mechanical projects, in particular in the construction of roads and highways
behaviour of these samples, (embankments, layer shapes, art works...).
The improvement by additions of physico-mechanical
properties of these elements, because there is a problem of
economic overhead, when their using in the raw state, so
there is a good normalization ( American standard, standard Benabbas Chaouki attachment Constantine University position Teacher
Researcher Degrees and diplomas: 1986 D.E.S. Hydrogeology option
AFNOR French and standard African which it's the lowest Consatntine University 1991 Ph.D Geology - Mineralogy Moscou
quality and cost). University 2006 Ph.D. in GeologyConstantine University The functions
occupied since the beginning of his career is Teacher since September 1991
ACKNOWLEDGMENT Continuation it's his way Manager of the Department of Earth Sciences from
1994 to 1997 then in parallel Teacher at the Ecole Normale Supérieure after
All authors thank, the Laboratory of Geology and that Director of the Laboratory "Geology and Environment," since Nov. 2006
Environment, LGE, Constantine University 1; the Process Currently he is the Manager of Master "Geology and the Environment", since
Engineering Laboratory, University of Bejaia and Birine September 2007 Courses taught General Geology - Geodynamics basins -
Tectonic Elements Pic-Interpretation.
Nuclear Center, Ain Ouassera, Algeria for their
collaboration.

REFERENCES Ait Abdelouahab Djaouza attachment Constantine University position

course instructor. Degrees and diplomas of 1984 Mining Geology,
[1] O. Kaufmann, A. Binni, and Co, “Microscopic study of „ghost‟ rock University of Constantine. Magister Mining Geology entitled: "Study of
weathering residues,” Acte Du Colloque Kast vol. 99, 1999.
metallogenic some Pb-Zn deposits in the north-east of Algeria (high plains of
[2] A. E. Bied, J. Sulem, and F. Martineau, “Microstructure of shear zones
Constantine)" supported at the University of Constantine. February 1996.
in Fontainbleau sandstone,” International Journal of Rock Mecanics
and Mining Sciences, vol. 39, pp. 917-932, 2002.
[3] J. F. Gamond and M. Mlynarczuk, Studia Geotechnica et Mechanica
no. 1-2, 2008.

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