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https://doi.org/10.1007/s12633-019-00109-5

ORIGINAL PAPER

Spectroscopic Characterizations of Sand Dunes Minerals of El-Oued

(Northeast Algerian Sahara) by FTIR, XRF and XRD Analyses
Nassima Meftah 1 & Mohammed Sadok Mahboub 1,2

Received: 4 November 2018 / Accepted: 12 February 2019

# Springer Nature B.V. 2019

Abstract
This paper investigates the chemical and crystal structural properties of sand dunes of El-Oued region from the northeast Sahara
of Algeria. By using of Fourier-transform infrared (FT-IR) spectroscopy, X-ray fluorescence (XRF) and X-ray diffraction (XRD)
we show that El-Oued sand dunes are composed mainly of 97.6% α-quartz (SiO2) and 0.56% calcite (CaCO3). Very low
concentrations of some oxides as Al2O3, Fe2O3, MgO and trace elements impurities were also found. The calculated crystallinity
index CI = 0.975 confirm the highly crystalline nature of quartz. From the X-ray diffraction data, structural parameters of quartz
and calcite minerals were determined. Quartz grains were found to have a hexagonal crystal structure with lattice parameters of
a = b = 4.907 Å and c = 5.401 Å and calcite grains have a trigonal crystal structure with a = b = 4.977 Å and c = 17.04 Å. The
calculated lattice parameters were similar to those of standard references. The crystallite sizes of quartz and calcite were estimated
to be nanometric.

Keywords Sand dunes . Quartz . Calcite . X-rays diffraction . Fourier-transform infrared . Structural parameters

1 Introduction chemical compounds [7]. Although the components of sand

grains depend on the local rock sources and conditions, the
In recent years, the interest in raw materials has increased main mineral constituents of sand are quartz (SiO2), feld-
due to their physico-chemical properties and also their spar (KAlSi3O8, NaAlSi3O8, CaAl2Si2O8) and carbonates.
availability. Sand of particular interest; it is widely used in In addition, it contains considerable concentrations of alu-
industry and nanotechnology [1]. The sand in its raw state is minum oxide (Al2O3) and iron oxide (Fe2O3), as well as
used in various fields: as building materials, thermal energy small amounts of heavy materials [8, 9]. Furthermore, sand
reservoir medium, water filtering material and in bricks and represents the most promising resource of quartz (silicon
ceramic manufacture [2–4]. Sand is defined as loose gran- dioxide) material compared to crystalline hard rocks.
ular material derived from weathering and natural disinte- Today, high-purity quartz has become a vital mineral, with
gration of rocks and other materials on the earth’s surface its particular physicochemical properties being employed in
and has grains ranging from 0.0625 to 2 mm in diameter [5]. a wide range of nanotechnologies such as glass fabrication,
The compositions and texture of sand grains are controlled optics and microelectronics, semiconductors and telecom-
by the chemical and physical processes such as wind action, munications [10–12]. Also, quartz contains Silicon (Si),
fluvial and marine processes, weathering, precipitation, and which can be exploited in various fields, including medi-
air temperature [6]. The sand can acquire various colors cine, sensor and biosensing, photonics, microelectronics,
ranging from light red to black due to the presence of certain energy technologies and solar silicon applications
[13–16]. Extracting quartz from sand or extracting silicon
from quartz and determining its suitability for different in-
* Nassima Meftah
dustrial applications require knowledge of the physical and
meftahnassima@yahoo.fr chemical properties of the quartz. Several investigations
have been undertaken on sand dunes from different regions
1 of the world. Howari et al. [17] have studied the geomor-
Department of physics, Faculty of Exact Sciences, University of
El-Oued, 39000 El-Oued, Algeria phology and mineralogy of different dune types in the east
2 Abu Dhabi using Landsat 7 ETM+ data sets. Trabelsia et al.
LEVRES Laboratory, Faculty of Exact Sciences, University of
El-Oued, 39000 El-Oued, Algeria [18] identified the physicochemical proprieties of Douiret
 Silicon

Fig. 1 Map of Algeria (http://

www.primap.com/wsen/Maps/
MapCollection/NationalMaps/
Algeria-Satellite-4000x3816.
html) showing El-Oued region
location and the dune from which
the analyzed samples are taken

sand in order to promoted the production of silica gel. Elipe Several studies have characterized the Algerian sand dunes,
and Lopez-Querol [19] characterized and improved aeolian but a very limited number thereof addressed the microscopic
sand for its potential use in construction. However, the and crystallographic properties of sand dune minerals.
existance of impurities on Tihimatine Quartz, Algeria has Algerian Sahara has enormous quantities of sand dunes
been characterized [20]. Also, some researchers have eval- (about a quarter of its total area). Moreover, it has very large
uated the quartz sand occurrences of the Santa Maria Eterna sunny areas making it a potential reservoir of solar energy.
formation, in northeastern Brazil, as a potential source of The El-Oued region is situated in the northeast Sahara
raw material for silica glass production [21]. Bennefi et al. of Algeria and is entirely covered by sand dunes.
[22] investigated the morphology, mineralogy, geochemis- However, quartz in its sand dunes, which has a great eco-
try, and provenance of sand dunes in Saudi Arabia. Adnani nomic importance, has not been characterized up to now.
et al. [23] have studied the color differences of sand dunes We assume that a good knowledge of the physico-
and then investigated sand’s origin and transport pathways. chemical properties of El-Oued sand and its components
The heat effect on the composition of dunes sand of Ouargla can contribute to exploiting this natural resource, in par-
region (Algeria) using XRD and FTIR has been studied ticular for the production of solar energy.
[24]. Recently, a study has characterized the desert sand of The aim of this study is to identify the minerals of El-
the United Arab Emirates which will be used as a thermal Oued sand dunes, assess the presence of pure quartz in the
energy storage medium in particle solar receiver technology sand dunes of this region and determine some crystal
[25] and other researchers carried out a mineralogical anal- structural properties of sand components, by using nonde-
ysis of sand roses and sand dunes samples from two differ- structive instrumentation such as Fourier-transform infra-
ent regions of South Algeria [26]. red spectroscopy (FT-IR), X-ray fluorescence (XRF) and
X-ray diffraction (XRD).

2 Materials and Methods

2.1 Geology Setting

El Oued region is located in northeast of Algeria Sahara has

border with Tunisia from the east (Fig. 1). Its geographical
coordinates are: latitude of 33°27′20″ North, longitude of
7°11′ 0″ East. This region is very sunny and its southern half
is covered by the Grand Erg Oriental, a vast region of unin-
terrupted sand dunes, and the rest is a mixture of sandy desert
with scarce vegetation, scattered oases, and salt lakes. In order
to ensure the quality of the results, samples were collected
Fig. 2 Micrograph of the El-Oued sand dunes from unmodified pristine dunes and away from engineering
Silicon

Table 1 Physicochemical
properties of the El-Oued sand Bulk density (g/ml) pH Porosity (%) Conductivity (μS/cm) TDS (mg/l)
sample
Sand sample 1.6 9.3 34.09 130.1 59

construction areas. About seventy-five samples were collected 3 Results and Discussion
from dunes located at the south of El Oued (33°8′54′′ north,
6°5′ 37.7 ′′ east). Samples were picked up from different faces Our sand sample has a beige color and its grains have
of the dune, from the top to bottom and at different depths. To shapes ranging from round to elongate to irregular as
homogenize the sampling protocol, equal weights well-mixed shown in the optical microscope image (Fig. 2). Some
samples were obtained. physicochemical properties of examined sand are present-
ed in the Table 1. The low porosity of 34.09% confirms
that the El-Oued sand belongs to the fine class. The alka-
2.2 Sample Preparation line nature of the sample (pH > 7) suggests the accessibil-
ity of exchangeable cations as Ca2+, Mg2+, K+, Na+ and a
As a first preparation step before XRD, XRF and FT-IR anal- high content of carbonate ions in sand. Also, the high
ysis, the sand was crushed by using a glass mortar. Before FT- value of the conductivity and the total dissolved solids
IR analysis, 2 mg of the crushed sand were mixed carefully (TDS) strongly depend on the presence of dissolved salt
with 198 mg of dry potassium bromide (KBr). The mixture (e.g. NaCl, Na2SO4, MgSO4, ....) in the sand [27].
was then compressed to form a pellet of 13 mm diameter and
1 mm thickness. A Shimadzu FTIR-8300 machine running 3.1 Analysis by Fourier-Transform Infrared(FTIR)
under the spectral range (400–4000 cm−1) was used to identify
the constituent bonds of the sand samples. For X-ray fluores- The infrared absorption spectrum of the El-Oued sand dune
cence measurements, the crushed sample was compressed un- samples is illustrated in Fig. 3. From the FT-IR spectrum we
der high pressure for few minutes to form a measurable pellet. can identify the main component of our samples. Table 2 sum-
A Philips MagiX Pro-XRF instrument was used to carry out marizes the functional groups found in the sand. In the range
the measurements. To determine the crystallographic parame- of the high wavenumbers we see a high intensity absorption
ters of the sand samples we used X-rays powder diffraction by band at 3429 cm−1 which is due to stretching vibrations of
an AXRD Benchtop Powder Diffractometer. At room temper- hydroxyl groups (OH) [28, 29], a less intense band has been
ature, the diffractometer worked with a wavelength λCuKα1 = observed at 1616 cm−1, which is due to the twisting of H-O-H
1.54 A° under a voltage of 30 KeV and a current intensity of [30]. Also, three absorption bands have been observed at
20 mA. The data sets were collected from the scans with 2θ wavenumbers of 2511 cm−1, which are due to (CO 3)−2
running from 20° to 80°.

Fig. 3 FTIR absorption spectrum 100

of El-Oued sand dunes
80
2855
2924

2511
2361

60
Transmiance (%)

3429

40
1798
1875
1616

20
694
876
795
1427

779

0
459
1080

-20
3850 3350 2850 2350 1850 1350 850 350

Wave Number (cm-1)

 Silicon

Table 2 The main bands of IR

absorption and associated bond Band (cm−1) Bond (Vibration mode) Compound
vibration of El-Oued sand
3429 H-O-H (stretching vibration) Water
2924 C-H (stretching vibration) Organic Carbon
2855 C-H (stretching vibration) Organic Carbon
2511 (CO3)−2 (asymmetrical stretch and symmetrical stretching) Calcite
1875 Quartz
1798 (CO3)−2 (plane bending and symmetrical stretching combination mode) Calcite
1616 H–OH (stretching) Water
1427 (CO3)−2 (asymmetrical stretching) Calcite
1080 Si–O–Si (symmetrical stretching) Quartz
876 (CO3)−2 (out-of-plane bending) Calcite
779 Si–O (symmetrical stretching) Quartz
694 Si–O–Si (symmetrical bending) Quartz
459 Si–O–Si (asymmetrical bending) Quartz

asymmetrical and symmetrical stretching mode vibrations [8]. We notice that the quartz of the El-Oued sand samples does
The 1427 cm−1 wavenumber feature is due to doubly degen- not contain other impurities suggesting a high degree of purity
erate asymmetric stretching mode vibration, and the 876 cm−1 for this sand quartz. In contrast, Beddiaf et al. [28] and
one corresponds to the C=O stretching mode vibration [8]. Maazouzi et al. [35] found that the Western Erg sand
These bands confirm the presence of calcite in our samples and the Ouargla sand in the Algerian Sahara have a con-
[31, 32]. A sharp absorption band at 1080 cm−1 has been siderable amount of Al2O3 and Fe2O3. The presence of
observed and seems to fit with symmetrical stretching of Si– the double absorption at 795 and 779 cm−1 is an indicator
O–Si bond [33]. In the spectrum range of 1080–400 cm−1 a of the presence of the quartz in α-phase [36, 37]. The
strong band has been observed. Symmetrical bands at 795 and crystallinity index (CI) of quartz in our sample is calcu-
779 cm−1 have been observed and correspond to Si-O sym- lated by measuring the ratio between the absorbance of
metrical bending vibration. These peaks confirm the presence the bands 795 and 779 cm−1 (A795/A779), where the ab-
of quartz [33]. In addition, we observed other bands at 694 and sorbance Aα at wavenumber α is defined as [38]:
459 cm−1 which coincide with Si–O–Si symmetrical and
asymmetrical bending, respectively. The presence of Si-O Aα ¼ −log T α ð1Þ
and O-Si-O vibrations in our sample again confirm the pres-
ence of quartz. The 694 cm−1 band indicates that the quartz in where Tα is the transmittance at wavenumber α.
our samples is crystalline [34]. Thus, FT-IR absorption spec- We found that the degree of crystallinity of sand quartz is
trum exhibits only an absorption band characterizing quartz equal to 0.975. Since the crystallinity index is inversely propor-
(SiO2) and calcite (CaCO3) compounds in our sand samples. tional to crystallinity of materials [39, 40], the calculated ratio

Table 3 Chemical analysis of El-

Oued sand dunes sample by X- The concentrations in (%) of oxides The concentrations in (ppm) of trace elements
ray fluorescence
SiO2 97.63 Cl 425
MgO 0.613 Zn 44.0
CaO 0.564 Ba 21.0
Na2O 0.542 Sr 6.00
Al2O3 0.327 Nb 5.00
CO2 0.105 Bi 5.00
K2O 0.0677 Ge 3.00
Fe2O3 0.042
SO3 0.037
P2O5 0.0138
TiO2 0.0053
MnO 0.0021
Silicon

Fig. 4 The XRD pattern of El- 4400 Q(011)

Oued sand dunes Q: Quartz mineral (SiO2)
3900 C: Calcite mineral (CaCO3)

3400

Intensity (Counts)
2900

2400

1900

Q (100)
1400

Q (112)
Q (102)

Q (121)
900

Q (203)
Q (122)
Q (110)

Q (200)

Q (022)
C (104)

Q (201)

Q (013)

Q (213)
Q (111)

Q (220)
Q (302)
C (0012)
Q (113)
C (116)

Q (104)
400

-100
20 25 30 35 40 45 50 55 60 65 70 75 80

( °)

indicates that El-Oued sand quartz has a highly crystalline our sample has a high concentration (97.63%) of silica, low
nature. concentration of calcium oxide (0.56%) and very low percentage
of aluminum oxide and iron oxide. A small amounts of MgO
3.2 Chemical Analysis by X-Ray Fluorescence (XRF) (0.61%) and Na2O (0.54%) have been noticed. Also, very low
levels for others oxides were found in the sand dunes sample.
The chemical compositions of El-Oued sand dunes obtained by Furthermore, as shown in Table 3, the El-Oued sand contain
XRF measurements are summarized in Table 3. We show that insignificant amount of other trace elements, such as bromine
(Br), germanium (Ge), bismuth (Bi), niobium (Nb), strontium
Table 4 Indexed Powder XRD Pattern for El-Oued Sand (Sr), zinc (Zn), barium (Ba) and chlorine (Cl). These results
Peaks 2θ(°) Intensity(a.u) Mineral (dhkl)cal (Å) hkl confirm that El-Oued sand dunes consist mainly of quartz with
minor calcite and very low quantities of Fe2O3, Al2O3, Na2O,
#1 20.89 1350 Quartz 4.434 100 SO3, MgO and TiO2. The very low concentrations of these ox-
#2 26.69 4300 Quartz 3.335 011 ides suggest the purity of the El-Oued sand quartz. The light
#3 29.49 270 Calcite 3.024 104 color of the sample results from the concentrations relatively
#4 36.59 340 Quartz 2.452 110 considerable of magnesium (Mg) and sulfur (S) in the El-Oued
#5 39.49 460 Quartz 2.279 102 sand dunes [34]. As well as the presence of Mg, Ca and K cations
#6 40.29 200 Quartz 2.235 111 contributed to increase the pH and the conductivity of sand.
#7 42.49 330 Quartz 2.125 200
#8 45.79 290 Quartz 1.979 201 3.3 Analysis by X-Ray Diffraction (XRD)
#9 48.60 120 Calcite 1.871 116
#10 50.09 590 Quartz 1.819 112 The XRD pattern of the sand samples is shown in Fig. 4. As is
#11 54.90 290 Quartz 1.670 022 evident, the diffraction peaks are related to the planes (100),
#12 55.30 130 Quartz 1.659 013 (011), (110), (102), (111), (200), (201), (112), (022), (013),
#13 60.10 270 Quartz 1.548 121 (121), (113), (122), (203), (104), (302), (213) and (220).
#14 64.09 100 Quartz 1.451 113 According to the JCPDS (N° 46–1045) standard pattern [41],
#15 65.59 80 Calcite 1.421 0012 these XRD peaks correspond to quartz with a hexagonal crys-
#16 67.79 410 Quartz 1.381 122 talline structure and belonging to the space group P3221 (154).
#17 68.29 450 Quartz 1372 203 We observed that the (011) peak has the highest inten-
#18 73.49 90 Quartz 1.287 104 sity indicating preferred orientation. Further, three other
#19 75.69 110 Quartz 1.255 302 peaks have been observed at 2θ = 29.49°, 48.6° and
#20 77.69 120 Quartz 1.228 220 65.59° which are related to (104), (116) and (0012) planes
#21 79.89 210 Quartz 1.199 213 respectively. These planes fit calcite (CaCO3) compound
as reported by JCPDS (N° 47–1743) with a rhombohedral
 Silicon

Table 5 Lattice parameters a, c and crystalline size D of quartz and calcite of El-Oued sand dunes

Mineral Standard lattice parameters (Å) Calculated lattice parameters (Å) FWHM (°) Crystalline sizes (nm) (D)

a Δa = a0-a c Δc = c0-c

Quartz (SiO2) a0 = 4.910 a 4.907 0.003 5.401 −0.001 0.2 42.64

c0 = 5.400 a
Calcite (CaCO3) a0 = 4.989 b 4.977 0.012 17.04 0.021 0.3 28.6
c0 = 17.061b
a
data from JCPDS (N° 46–1045)
b
data from JCPDS (N° 47–1743)

crystal system belonging to R3c (167) space group. We where D is the crystallite size, λ (=1.54 Å) is the wavelength
note that the majority of the crystallographic planes are of X-rays, β is the width full at half maximum (FWHM) of the
due to quartz SiO2 (Table 4), with the presence of three most intense diffraction peak, usually measured in radian and
planes belonging to calcium carbonate CaCO3. θ is the Bragg angle.
The XRD results agreed with XRF and FTIR spectroscopy The crystallite size of quartz D = 42.64 nm is very large
data confirming that the dominant phase in the sand dunes of compared to calcite size D = 28.6 nm, but remain less than
El-Oued is quartz (SiO2). 100 nm which makes it of great interest to the nanometric
The dhkl inter-planar spacing has been calculated from the industries and nanotechnologies.
X-ray diffraction profile using the Bragg law:

2d hkl sinθ ¼ nλ ð2Þ

where θ is the diffraction angle, λ is the used wavelength of X-

4 Conclusion
rays and n is the order of diffraction. We note that the calcu-
The sand dunes of El-Oued region were characterized using
lated value of dhkl-spacing (Table 4) matched very well with
FTIR spectroscopy, XRF and XRD analysis. We found that the
those of the standard JCPDS data. From Table 4 the spacing
El-Oued sand mainly consists of about 97.63% quartz in α-
distances dhkl of 4.43, 3.33 and 2.45 (Å) affirm the presence of
phase, minor calcite mineral (about 0.56%) and very low con-
the α-quartz phase in our sand [28, 33]. The α-quartz is the
centrations of other oxides (Al2O3, Fe2O3, Na2O, MgO) and
most stable phase of quartz at room temperature. The lattice
some trace elements. The low quantities of the impurities bear
constants a, b and c, for the hexagonal phase structure were
witness to the high purity of the quartz sand of El-Oued region.
determined from XRD results using the following equation:
The degree of crystallinity of our sand quartz has been estimated
to CI = 0.975, which supports the high crystalline nature of the
 
1 4 h2 þ hk þ k2 l2 quartz. The XRD analysis corroborate that our sand is very rich
¼ þ ð3Þ in quartz with hexagonal crystal structure and belonging to space
dhkl 2 3 a2 c2
group P3221 (154). Furthermore, the sand has some calcite with
where (h k l) are the Miller indexes and ‘a’ and ‘c’ are the trigonal crystal system and R3c (167) space group. We estimated
lattice constants. the crystallite size of quartz to D = 42.64 nm, which demon-
The calculated and standard JCPDS lattice constants for strates the nanometric aspect of the El-Oued sand quartz.
quartz and calcite are indicated in Table 5. As we can see, the
calculated lattice parameters for the quartz (a = b = 4.907 Å and Acknowledgments We greatly appreciate the constructive comments of
c = 5.401 Å) agree well with the standard values (a0 and c0). the reviewers. The authors are grateful to S. Mostefaoui from the
University of Pierre et Marie Curie, Paris for his beneficial discussions
Since impurities in the crystal lattice would affect the d- and suggestions to improve the manuscript and we are very thankful to M.
spacing between lattice planes and therefore the lattice param- Telus from the University of California Santa Cruz, USA for his help in
eters, the above agreements confirm the high degree of purity improving the language of this manuscript.
of quartz of the El-Oued sand dunes. We can further calculate
the crystallite sizes D of the quartz and calcite of our sand from Publisher’s Note Springer Nature remains neutral with regard to jurisdic-
tional claims in published maps and institutional affiliations.
the strongest peaks by using Scherrer’s formula [42]:
0:96 λ
D¼ ð4Þ
βcosθ
Silicon

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