Journal of Advanced Research in Science and Technology

ISSN: 2352-9989

Chemical and Physical Investigations on the barite of Ain

Mimoun ore deposit –Khenchela - North-eastern Algeria

K. Abdellaoui 1∗, A. Boumaza 1, N. Kamoun 2 , A. Boutaleb 3

1
Structures, Properties and Inter Atomic Interactions Laboratory (LASPI2A), Faculty of Science and
Technology, University of Abbes Laghrour, Khenchela 40000, Algeria
2
Université de Tunis El-Manar, Faculté des Sciences de Tunis Département de Physique, Laboratoire de
Physique de la Matière Condensée.Tunisia
3
Laboratoire de Métallogénie et du Magmatisme de l’Algérie, Faculty of Earth Sciences, USTHB,
Algiers 16 111, Algeria

Abstract. In this work, we are interested in the barite of Ain Mimoun of the region of the wilaya of
Khenchela-Algeria. This ore has not been chemically and physically studied before. This mineral is used in
various industries for its special properties: high density, chemical neutrality, whiteness and no abrasive. Among
which, it serves as a mineral filler in a wide variety of products including paints, paper, glass, rubber, plastics,
friction materials and barriers for protection against radiation. The Ain Mimoun barite deposit remains one of the
important sites for the production of barite primarily intended for oil fields as a weighting of the drilling mud.
For this purpose, various techniques have been deployed, such as X-ray diffraction (XRD), Fourier Transform
Infrared Spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), differential thermal (DTA),
Thermogravimetric (TG) analysis, and photoluminescence optical properties (PL). Various oxides and / or
hydroxides associated with this mineral have been found, especially oxides rich in silice, iron, zinc, copper, etc.
The estimation of the quantity of strontium in this barite was proposed in this work. The coexistence of
numerous minerals testifies to the richness of this study area.
Keywords: Barite; XPS analysis; FTIR analysis; TG-ATD analysis; Ain Mimoun ore deposit.

1. Introduction
Barite exist in various environments ranging from sedimentary to non-sedimentary (hydrothermal
and exhalative) conditions [1-2]. Barite is a common mineral in hydrothermal deposits, such it’s in the
Ain Mimoun ore deposit case. The Ain Mimoun ore deposit is located in the anticline of Djebel
Chentgouma, about 25km SW of Khenchela. The vein field occupies the northern flank of a large fold
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of NE-SW direction. It was discovered in 1968 during a systematic exploration of the region. During
the 1972-2005 years, the exploration and extraction in the deposit area have allowed the discovery of
new reserves and the entire deposit were estimated at 5.577 million tons barite ore. It is currently
mined by an open pit and underground operation. Despite its economic importance very little work has
been done on the origin of the Aïn Mimoun ore deposit and characterization of barite from this deposit
has never been studied. Nevertheless, we can cite the works cited in references [3], [4], [5], [6], and
[7].

*
Corresponding author.
E-mail: [email protected] (Abdellaoui K.).
Address: Université Abbes Laghrour, Khenchela 40000, Algérie

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Barite is one of the most important industrial minerals. It was noticed due to its high density.
Barium Sulfate (BaSO4) is suitable for many diverse applications because of its whiteness,
inertness and high specific gravity[8]. Given to its various applications, its large reserves and
its intensive use, it contributes significantly to the economic and industrial development of the
country. Barium sulfate is a kind of important inorganic chemical product as packing and
additive in painting, coating, plastics and medicines fibers [9-10-11]. Barite is one of the most
important fillers used in the plastics, rubber and paint industries, and is also used in
pharmaceutical formulations [12-13-14]. The field of use of this mineral is versatile, it
includes in oil drilling, hydraulic, battery industry and the chemical (paint) and fluoroscopy,
protective barrier against radiation, glassware, employed also in dense concrete, it is also used
as an inert filler in the friction materials such as brake pads and clutch disc. Among other
things, it can be used as a gas sensor for vacuum tubes, lubricant (additive), filler and paper
dye. To this end, the mining industry in Algeria is responsible for the operation of this type of
ore. Besides the barite veins, one meets several indices as the mineralization of copper, lead,
quartz, calcite, etc. Quartz (SiO2), the dioptase (CuSiO3, H2O), chalcopyrite (CuFeS2),
sphalerite (ZnS), Cinnabar (HgS), calcite (CaCO3), iron hydroxides (Fe2O3, H2O), and the
malachite and azurite (Cu2CO3(OH)2).This study is based on a set of experimental chemical-
physical techniques to characterize this mineral from the region of khenchela and also to
know the acolyte products. Thus we present and analyze the results of X-ray diffraction, XPS,
FTIR, and DTA-TG analysis.

2. Characterization of samples
All the samples are then characterized using XRD, SEM observations and qualitative
analysis, FTIR spectroscopy, XPS spectroscopy, and DTA-TG analysis.

-X-ray diffraction analysis is performed with a PANalytical X’Pert ProMRD diffractometer

with CuKα radiation ((λ(Kα1) = 0.15406 nm, λ(Kα2) = 0.15444 nm)). Data are collected with
steps of 0.021° (2θ).
-Scanning electron microscope SEM microscope (JEOL 7500-F) was used, equipped by
Genesis EDX spectroscopy system that was used to measure the composition of the elements
constituting the mineral.
-XPS analysis An XPS K-Alpha spectrometer was used to qualitatively and quantitatively
verify the composition of the different powder compounds. The spectra were treated using the
Thermo advantage V5.27 software. The photoelectrons are excited using a monochromatic
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Al Kα radiation as the excitation source, collected at θ = 0° with respect to the surface normal
and detected with a hemispherical analyze. The spot size of the XPS source on the sample is
200 µm, and the analysis is operated with pass energy of 150 eV for the survey spectra and 20
eV for the accumulation spectra of the core levels. The pressure is maintained below 1x10-8
Torr during data collection, and the binding energies (Eb) of the obtained peaks are referenced
to the C1s signal for C–H, which is set to 285.0 eV. XPS measurements are made with
uncertainties of about 0.2 eV.
- Fourier transformation Infrared spectroscopy (FTIR) IR spectra are obtained using a
Perkin–Elmer spectrometer at the resolution of 8 cm-1. Fourier transform infrared (FTIR)

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technique is used in the transmission mode in the 4000 - 400 cm-1 range. For each sample,
120 scans are used. After the oxidation, ~100 µg of the oxides are scraped. The oxide is then
compressed together with 23 ± 2mg of KBr in a cold 150 MPa isostatic press (CIP) in order to
obtain a 200 - 250 µm thick pellet. All infrared spectra are reporting absorbance (A= - log
(I/I0)) as a function of the incident wave numbers.
- DTA and TGA analysis , barite powders were subjected to differential thermal analysis
(DTA) and thermogravimetric analysis (TGA) using NETZSCH STA 409 PC/PG instrument,
with α-alumina as the reference material at a heating rate of 10°C/min in azote (flow rate 10
ml/min), sample mass was about 34 mg.
3. Experimental results
3.1. Macrographique observations, and EDX analysis
Barite mineral is soft but heavy, slightly tinged with white, gray, yellow or brownish. Barite is
a mineral species composed of barium sulfate BaSO4 formula with traces of Sr, Ca and Pb.
On hydrothermal origin, barite presents various compositions. Rich in Pb, Sr, C, Ra, or
several of these elements associated with them or other, dedicate this mineral to the multiple
uses. This mineral usually crystallizes as flattened crystals, sometimes lamellar. Crystals are
tabular, prismatic, and as grainy, platy, and coxcomb aggregates. Crystals may be present in
aggregates (typically cleavable), and these crystals are lenticular grouped into rosettes. Macro
graphic images are shown in Figure 1, and 2.

Fig.1: Photomacrograph of barite samples; massive barite-whitish (a), Platy tabular barite (b), barite crystal
rosette (c).
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Fig.2:The photomacrograph of the barite samples; inlaid barite,SiO2 (a, b), and blue spot known as the azurite
mineral (c).

In crystals, lamellar masses, fibrous, grainy and compact. This mineral contains SiO2 crystals
embedded in cavities (Figure 2a, and b). Blue spot are split in surfaces (azurite) as shown in
figure 2c.

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The SEM analysis (figure 3) confirms the presence of the various components of barite, in
this case we can draw Table 1, giving the molar percentages and mass percentages of Ba, O,
S, Si, Ca, Mo, Al, Zn, Ti, elements.

Fig. 3: The EDX spectrum of the raw barite-Ain Mimoun.

Table 1: The EDX analysis of BaSO4 (Ain Mimoun).

Element KeV Mass% Atom%
Al K* 1.486 0.30 0.46

Mg K* 1.253 0.31 0.52

Ti M 2.267 1.44 0.29

Ca K 3.690 1.48 1.49

Si K 1.739 2.24 3.22

Mo L 2.293 4.13 1.74

SK 2.307 10.73 13.50

OK 0.525 24.92 62.81

Ba L - Bal Bal
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3.2. X-ray diffraction analysis

Figure.4a. Shows the X-ray diffraction pattern of barium sulphate particles. For the
identification of crystal structure and the determination of the particle size, we used X-ray
diffraction. All the reflection plains are matched with a orthorhombic phase of barium
sulphate [15-16-17], with crystalline cell constants a = 7.144, b = 8.865 and c = 5.445A˚,
which are basically in agreement with the reported values (JCPDS Card Files No. 80-0512),
space group Pnma.

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Fig. 4: (a) The X-ray diffraction of barite, (b) X-ray (200) and (011) plans of various barite.

The coexistence of SiO2 is indicated by the peaks at 2θ = 26.6° and at 20.8°. The small peaks
between 29° and 31° may indicate the possible presence of small amounts of complex as
battlerite, Azurite, CaCO3, whose elements were analyzed by XPS and EDX, those
compounds in oxidized, sulphurised or hydroxide states.

The crystalline sizes of the natural barite are calculated using Scherer’s formula [18] for the
four high intensity peaks observed at 26.10°, 41.02°, 42.50°, and 44.37 °(2θ) with hkl values
(210), (221), (122), and (410). In a first approximation, the full-width at half-maximum β can
be expressed as a linear combination of the contributions from the crystallite size, D, and the
strain, ε, through the relation

cos( ) 1 4 sin( )
= +

With λ the X-ray wavelength and θ the Bragg diffraction angle. The values of β and θ
parameters are estimated by Gaussian fitting of the XRD peaks. In order to improve the
statistics, the (210), (221), (122), and (410) diffractions peaks of barite was used. Results of
calculations are given in table 2.

Table 2 : The crystallite size and strain of barite.

Parameter Crystallite size (nm) strain
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Values 54.53 ± 10.12 0.27±0.05

Qualitative estimation of the amount of SrSO4 by X-ray diffraction:

Qualitative estimation of the amount of SrSO4 in barite was calculed by X-ray diffraction
[19]. The molar amount of SrSO4 is possible using this technique. Ratio study of the
intensities of the (200) and (011) plans based on strontium content in barite (figure 4b). It was
reported by the reference [19] that the intensity of the (011) line decreases with increasing
strontium content in barite, finally for 25% higher contents, this peak will confound the (200)

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 Abdellaoui K. et al., Journal of Advanced Research in Science and Technology, 2019, 6(1), 865-877.

peak. The lines (011) and (200) are shown in figure 4b this reference even gives the
relationship.

Y = 0, 6. X + 1.7

Y being the value of the ratio I(011) / I(200), and X is the mole percentage of SrSO4 in barite.
The measure allows the report to determine the content of SrSO4. For a mineral without
CuSO4, we have Y= 0, various powders of barite were used, we give the results of the
intensities ratios and the percentages of SrSO4 in mol percent in the table below.

Table 3 : The SrSO4 estimation.

Powder-1 Powder -2 Powder -3 Powder -4 Powder-5

(011) area 8.73 86.28 88.06 55.59 59.57

(200) area 109.31 178.88 173.77 125.09 147.08

SrSO4 mole 0.26 0.62 0.45 0.91 1.28

percent
Average value of
SrSO4 mole 0.79 ± 0.37
percent

3.3. XPS analysis

Figure 5a shows the XPS survey spectra of the raw barite. For this mineral, the spectrum
reveals photoemission peaks for O1s, C1s, S2s, S2p, Ba4d, Ba4p, Ba4s, Ba3d, Ba3p and Ca,
which indicates the presence of O, C, S, Ba and Ca on the surface of this compound. The
related XPS analysis (Fig. 5a) shows that the binding energies of Ba 3d, S 2p and O 1s are
~778 eV, ~170 and ~531eV, respectively, close to the values of BaSO4 reported in the
literature [20-21]. Furthermore, the analysis result also exhibits the atomic percent of Ba, S,
O, Ca, and C adventious.
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 Abdellaoui K. et al., Journal of Advanced Research in Science and Technology, 2019, 6(1), 865-877.

Fig. 5: (a) The XPS spectroscopy of barite (Ain Mimoun-Khenchela), (b and c ) XPS spectroscopy of barite core
levels of Ba3d and O1s respectively.

The table below gives an estimate of the molar amounts of the elements on the surface of the
barite.
Table 4 The Atomic percent of BaSO4 by XPS analysis.
Name PeakBE (eV) FWHM (eV) Area(p) Atomic %
CPS*eV
Ba3d 778 3.78 2358220 12.72

O1s 531 3.85 1612000 44.24

C1s 285 4.01 287318 29.09

Ca2p 346 5.68 56184 1.15

S2p 170 3.19 229896 13.11

It can be seen from figure 4b, that the double peaks for Ba element are at ~780 eV (Ba3d5/2)
and ~794 eV (Ba3d3/2), and the binding energies are consistent with the standard values of
Ba in BaSO4 [20-21]. The peak around 780 eV can be divided into three peaks at 780.8,
777.9, and 774.4 eV, this type of profile was cited in references [22-23]. The O1s (figure 5c)
the energy band can be also divided into three peaks at 531.8, 529.7, and 525.5 eV. These
various values of energies reveal the complexity of states (oxides, hydroxides and sulfides) in
the raw barite.
Other elements in small amounts can be detected, so we can identify the bands of Si, Zn, Fe,
Ti, Na, and also Sr [24-31].
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3.4. FTIR Spectroscopy

We analyzed various forms of barites and different parts of this mineral. The spectra obtained
can identify not only the barite, but all acolytes compounds. These analyzes were highly
effective, in fact we were able to identify all the minerals and oxides present in the
environment of the barite.

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The spectra show no ambiguity, and reveal the power of this technique. Figure 6a-b shows
FTIR spectrum of BaSO4. In this figure many bands can be observed at 3450, 2924, 2850,
2061, 1632, 1384,1180, 1116, 1084, 982, 878, 800, 880, 634, 610, and 474 cm-1. The results
are in agreement with those reported in bibliographic data [32-33]. This barite also contains
quantities of silicates, azurite, and other minerals revealed in the following figures.

Fig. 6: (a-b) The FTIR spectra of various states of barite (Ain Mimoun), (c) FTIR spectra of SiO2
embedded in barite, (d) FTIR spectra barite, barite with azurite, and azurite embedded in barite.

The spectrum in figure 6c is relative to the quartz present in the masses of barite. This
silicon oxide was removed from the home in barite and then analyzed. In this figure many
bands can be observed at 3452, 1622, 1384, 1166, 1082, 796, 778, 694, and 458 cm-1 [34-35].
Figure 6d revealed the specter of azurite which is found left as blue spots on the barite (the
ore was taken from barite and analyzed). In addition to quartz, azurite, various parts FTIR
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Specters can confirm the existence of the butlerite (Fe(SO4)(OH) .2H2O), M-OH with
hydroxides (M = Fe2+ , Mg2+ ..), ZnO, and dolomite, Sodium and potassium sulfates (NaSO4-
KSO4) are both measured at 619 cm-1, for Na2SO4 and K2SO4 the peak correspond to the ν4
vibration [36-46].

3.5. DTA-TG Analysis

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 Abdellaoui K. et al., Journal of Advanced Research in Science and Technology, 2019, 6(1), 865-877.

The curves representing the behavior of barite under temperature; TG and DTA are shown in
figure 7. Heating was performed from 25°C up to 1400°C. Between room temperature and
200°C, thermogram indicate low weight loss less than 0.16%, which corresponds to the
endothermic phenomenon of loss water of hydration (of barium compounds, quartz, and
azurites hydrated) and that of any organic matter transformations. Between 200 to 782.7 °C, the
TGA thermogram indicate low mass gain of 0.42%, which can be attributed to a low oxidation during
this treatment. Between 785.7 and 830°C, the thermal images ATG indicate a mass loss less than
1.4%, which corresponds to the endothermic dehydroxylation phenomenon in compounds contained in
barite. At 1169 °C, barite begins its decomposition into BaO. Continuing the slope of the figure
corresponding to the TG curve, this decomposition becomes complete between 1550 and 1600 °C.
The complete transformation corresponds to a loss of mass equal to 34.30% [47-52].

Fig. 7: The DTA and TGA curves of barite (Ain Mimou).

The presence of SiO2 in significant quantity, small amount of CaCO3, and other compounds
as analyzed by FTIR, may lead to some disruption DTA and TG behavior of figures. This
around ~ 462.4°C, there is an endothermic phenomenon without loss of mass that
reflects the polymorphic transformation of alpha-quartz to α-quartz [53-55].
The presence of dolomite may also cause some processing related to the passage of
MgCa(CO3)2 to give as MgO in the first stage (550-750°C), and CaO in the second stage
(870-960°C) [56- 58].
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3.6. Photoluminescence spectroscopy

During this study the PL properties of the barite was measured with an excitation wavelength
of 266 nm. The figure 8a gives the normalized PL spectra of the mineral.

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 Abdellaoui K. et al., Journal of Advanced Research in Science and Technology, 2019, 6(1), 865-877.

Fig. 8: (a, and b) The PL spectrum at room temperature related to the barite of Ain mimoun, excitation
wavelength used λexc = 266 nm.

The characteristic peaks extend into the wavelength region between 370 and 600 nm,
signaling that the most intense peaks are between 380 and 550 nm (figure 8b).
Upon 266 nm excitation, a typical PL spectrum consists of several emission peaks:

- Intense violet bands having peaks 380 nm, and 421nm,

- The spectrum also includes blue intense band at 485 nm,
- And the less intense green band at 529 nm.
The origin of these emissions may arise either from intrinsic defects or/and extrinsic defects.

-a- Intrinsic defects

The main intrinsic defect type in oxides (Al2O3, ZnO, TiO2, etc…) is oxygen vacancy; called
F centers (Fabre or color center) and it is known that, in the presence of F type defects, UV
and visible emission are obtained from the matrix depending on the type of the F centers [59-
60-61]. Defects induced in oxides may be of various kinds:
-F centers (oxygen vacancy with two electrons),
-F+ centers (oxygen vacancy with one electron),
-F2 centers (two oxygen vacancies with four trapped electrons),
-F2+ centers (two oxygen vacancies with three electrons),
-And F22+centers (two oxygen vacancies with two electrons) [62].
Also, Ali+ centre, which consist of an interstitial aluminium ion having the charge of +1, has
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been found in α-Al2O3 with emission at 2.4 eV (516.5 nm) in PL spectroscopy [63].

-b- Extrinsic defects

Optical properties of oxide solids are also influenced by metal ions (extrinsic defects), which
can appear in quantities below 0.1 wt.%. Ions with an incomplete 3d shell (Ti3+, Cr3+, V3+,
Mn4+, Fe3+, Ni3+) substitute for Al3+ ions in the α-Al2O3 lattice [64-65-66].

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 Abdellaoui K. et al., Journal of Advanced Research in Science and Technology, 2019, 6(1), 865-877.

According to literature information, we can assign the bands at 380 nm (3.26 eV), 421 nm
(2.95 eV), and 485 nm (2.56 eV) to the intrinsic defects corresponding to the oxygen
vacancies, and the weaker band at 529 nm (2.34 eV) to possible extrinsic defects.

4. Conclusion
Barite is a common mineral in hydrothermal deposits, which is the case of the Ain Mimoun
deposit. It is a mineral that plays a very important role economically, it is found in petrology,
chemistry, glass, automotive, paper, medicine, etc. In our work we have characterized this
mineral by X-ray diffraction, XPS, FTIR, and also realized thermal analyzes DTA-TG.
Physico-chemical analyzes confirmed the coexistence of minerals such as silica, azurite, and
dolomite. These encrustations and various oxides, hydroxides, sulfides and carbonates closing
elements such as Fe, Zn, Sr, Ti, Ca, Mg, Mo, and Al. The amount of SrSO4 was estimated by
X-ray diffraction. Finally, the results of photoluminescence show a predominance of intrisic
defects due to oxygen vacancies.

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