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ANALYSIS OF SOIL, WATER ANDDUST DURING LIMESTONE MINING AND

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 ANALYSIS OF SOIL, WATER AND
DUST DURING LIMESTONE MINING
AND PROCESSING

AKANDE, J. M. and IFELOLA, E. O.

Department of Mining Engineering
School of Engineering and Engineering Technology,
Federal University of Technology,
Akure, Ondo State, Nigeria.
E-mail: seyfel2k4@yahoo.com,
akandejn@yahoo.com

ABSTRACT
Soil and water from the surroundings of a growth on them. Water samples from within
limestone mining and cement producing the mine’s premises and post-effluent discharge
company situated in Ogun State, South Western points along the receiving water bodies (stream
Nigeria were sampled and analyzed. Kiln- and river) were slightly alkaline with pH ranging
generated dust was also collected and analyzed. from pH(7.0-7.5). Hardness, conductivity, TDS,
Environmental quality parameters to determine and Fe2+ contents of effluent from raw mill
the nature and extent of influence of exploitation section were comparatively high having values of
and processing activities were carried out on 180mg/l, 5.4x102(μmhos), 250mg/l and 6.2ppm
the obtained samples. Data obtained from respectively. Analysis of dust from the factory’s
soil and water were compared with controls two kilns revealed that an estimated 28.22tonnes
(samples collected from undisturbed areas) of dust containing about 58% of calcium oxide
and with Food and Agricultural Organization (CaO) and 13% of Silicon oxide (SiO2) is generated
(FAO), World Health Organization (WHO) and from the kilns on hourly basis. Thus, in order to
Federal Environmental Protection Agency (FEPA) avert unpleasant consequences, the efficient
standards. Results showed that soil organic matter operation of the incorporated dust- trapping
ranged between (0.24-2.89) percent for all soil mechanism (i.e. electrostatic precipitation) is
samples. Primary macronutrients (N, P, and K) in imperative to keep the ambient atmosphere from
soil were between (0.01-0.15) %, (1.12-2.05)mg/ being constantly polluted.
kg and (0.01-1.03) Cmol/kg respectively. There
was a significant deficiency of organic matter Keywords: Limestone, Exploitation, Soil, Water,
in samples from dust dump and reclaimed land Dust, Effluent, Quality parameters, Cement,
sites indicating sparse or absence of vegetative Environment

ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011 15

1. INTRODUCTION ceased. Similarly, the action of rainwater on piles of
mining waste (tailings) where applicable, transfers
Modern mining is an industry that involves the
pollution to freshwater supplies. Water supply is said
exploration for and removal of minerals from the
to deteriorate when there is diminished quantities of
earth, economically and with minimum damage to
groundwater and surface water or deterioration in its
the environment (Michael, 2010). However, mining
quality. As noted by (FAO, 2003), poor quality water
causes physical disturbances to the landscape, thus
may result not only from inappropriate land use and
creating aesthetic eyesore such as waste-rock piles
soil management practices which result in material
and open pits. Such disturbances may contribute to
transport by surface runoff but also from industrial
the decline of wildlife and plant species in an area.
pollution due to inadequate processing controls.
Land degradation arising from human-induced
Changes in land use that reduce the protective
(anthropogenic) or natural process impairs the
ground cover and decrease surface soil porosity,
capacity of land to function and soils are the critical
such as inadequately-managed conversion of forest
component in land degradation when it involves
vegetation lead to increased runoff.
acidification, contamination, desertification, erosion
Surface mining operations present dynamic and
or salination (Johnson et al, 1997). Usually, in surface
highly variable silica dust sources. Dust particles below
mineral exploitation, landmasses are disturbed through
10µm are called respirable dusts and are generally
clearing or removal of vegetation, in the process, top
airborne (Farmer, 1999). Most of the dust generated
soil which contains 1-3 percent of organic carbon and
at surface mines is produced by mobile earth-moving
nutrients essential for plants growth are removed and
equipment such as drills, bulldozers, trucks, and front-
in most cases destroyed (Akande and Idris, 2003). Soil
end loaders excavating silica-bearing rock and minerals.
is a living, dynamic ecosystem. Healthy soil is teeming
Overexposure to airborne respirable crystalline silica
with microscopic and larger organisms that perform
dust could cause silicosis, a serious and potentially
many vital functions including converting dead and
fatal respiratory lung disease (NIOSH, 2010). Farmer
decaying matter as well as minerals to plant nutrients.
(1993b) remarked that the impact of dust depends on
Different soil organisms feed on different organic
its composition, particle size and concentration. The
substrates and their biological activity depends on
manufacturing of cement involves mining; crushing
the organic matter supply. Soil organic matter – the
and grinding of raw materials (mostly limestone and
product of on-site biological decomposition – affects
clay); calcinating the material in rotary kiln; cooling
the chemical and physical properties of the soil and
the resulting clinker; mixing the clinker with Gypsum;
its overall health. Its composition and breakdown
and milling, storing and bagging the finished cement.
rate affect: the soil structure and porosity; the water
This cement manufacturing process generates lot of
infiltration rate and moisture holding capacity of soils;
dust, which is captured and recycled to the process
the diversity and biological activity of soil organisms;
(Partha, 2008). Cement dusts are toxic; sometimes
and plant nutrient availability (FAO, 2005). Various
containing chromium which is carcinogenic (Fabbri
types of human activity such as clearing of vegetation;
et al, 2002). The mineral content of cement dust
decrease soil organic matter contents (Curry and
slows down plants growth rate while the alkalinity and
Good, 1992).
mineral content of dusts increase water pH. Also the
Brady and Weil (1999) list eighteen (18) soil
alkalinity of limestone dust contributes to raise the
nutrients essential for plants. They are classified into
soil pH of acidic or neutral habitats resulting in loss of
four groups; major non-mineral macronutrients, these
plants and animal species (Farmer, 1993b).
are 90% -95% dry plant weight, and are supplied to
Wet process of cement production requires large
the plant by water absorption and photosynthesis, i.e.,
volumes of process water resulting in slurry production.
C,H,O; primary macronutrients, i.e., N,P,K; secondary
Slurry from settlement ponds could leak into the
macronutrients, Ca, Mg, S and micronutrients, i.e., B,
adjoining drains as turbid water, polluting the natural
Cl, Co, Cu, Fe, Mn, Mo, Ni, Zn. Soil pH can affect
water courses of the receiving streams. Randall (1970)
the type and amount of anions and cations that soil
and Knut (1983) noted that high turbid water inhibits
solutions contain and can exchange with the soil
penetration of light, hence, retards or prevents proper
atmosphere and biological organisms(Dan, 2000).
growth of algae, which are primary food for planktons
According to (Mark, 2005) mining causes water
in the food chain of aquatic lives.
pollution in a number of ways broadly classified into
In view of the aforementioned, this paper aims
two sources- ‘‘point source and non-point source”. One
at evaluating some environmental-related soil,
of such pollution is the exposure and leaching of heavy
water and dust indices of limestone exploitation
metals and sulfur compounds that were previously
and processing at a cement producing factory. The
locked away in the earth by rainwater, resulting in
factory is located in Shagamu, Ogun State about 45
«acid mine drainage» and heavy metal pollution that
km from Lagos in the South-Western part of Nigeria
could continue long after the mining operations have
.Its raw material (limestone) is extracted from an
16 ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011
open pit mine close to the cement factory. The into a nearby stream which empties into a river
company employs wet method which utilizes great (Odan river). Figs.1 shows Nigeria while Fig.2 shows
amount of water to produce cement from limestone Shagamu the study area indicated as an inset within
and disposes off the excess or used one as effluent Ogun State.

MATERIALS AND METHODS transferred into 50m1 beakers. Distilled water 20m1
was added to each weighed sample and stirred with
Soil sampling and parameter determination glass rod for about 3 minutes. It was then left for 30
Soil and water samples as well as dust data were minutes to settle. The pH levels of the samples were
collected from the surroundings of the Mining measured by inserting the probes (electrodes) of
Company. Five soil samples labeled S1-S5 were already calibrated pH meter into the supernatant in
collected from specific locations within and outside the beaker (ICARDA,2001) and taking the readings.
the mine. Each sample weighing between (1-2) kg
Determination of Nitrogen using regular Micro-
was scooped within 0-20cm depth (Rao and David,
Kjeldahl Method
2007; ICARDA, 2001 ) and put in polyethylene bag
before taking them to the laboratory for analysis. Air–dried, 2mm-sieved soil samples weighing 1.0g
Parameters such as organic matter content, soil were transferred into 500ml micro – Kjedahl flask.
nitrogen, soil available phosphorus, potassium, Distilled water 20ml was added and swirled for few
calcium, magnesium, sodium and pH were according minutes and left for 30 minutes. Concentrated H2S04
to( ICARDA, 2001) examined. (20ml) and one tablet of copper oxide catalyst were
also added. The samples were digested at 3200C for 5
Soil Sample Designations based on collection Sites: hours. The flasks were removed and allowed to cool.
S1: Soil sample from reclaimed land The digests were then decanted into other micro
S2: Soil sample from virgin (unstripped) land Kjedahl flasks; 100ml distilled water was added to
S3: Soil sample from Odan river bed just before factory decant in flasks and individually attached to distillation
effluent discharge apparatus. 10ml of 40% NaOH solution was added.
S4: Soil sample from cement mill vicinity beside factory Then 5ml boric acid (H3BO3) with indicator solution
main access road was transferred into a 250ml conical flask placed
S5: Soil sample from dust dump under the distillation apparatus. With the condenser
tip about 4mm above the surface of boric acid solution;
Soil Analysis the digest was distilled by allowing hot steam pass
Soil Preparation: All soil samples were first air-dried, from steam pot thereby causing the digest to volatize
ground and sieved. and distil over the boric acid till about 50ml distillate
was collection. The distillate was titrated against 0.5m
Determination of pH: standard HCl. The colour at end point was green to
pink( Bremner and Mulvaney, 1982; AOAC,1990).
Ten (10)g of air–dried soil sample were weighed and
ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011 17
Phosphorous determination Water Sampling and Determinations
A sample of 5g air-dried, 2mm mesh-sieved soil A total of eight water samples were collected within
was weighed into beaker and 35m1 of phosphorous and outside the mine. Distilled water–rinsed 1-litre
extracting solution NH4C1 was added. The mixture plastic containers were used. Before final collection,
was stirred for 15 minutes and filtered by whattman each sample container was pre-rinsed three times with
No 40 grade (100mm). Ascorbic acid and ammonium sample water. Samples were then collected by dipping
molybdate reagents were added to 4ml of filtrate. the containers’ mouths deep beneath the water
Distilled water (5m1) was added and the solution was surface at the centre of water flow and filled to brim.
allowed to rest for 30 minutes for colour development Thereafter the samples were corked and taken to the
(i.e. blue). The standard was prepared by measuring laboratory for immediate analysis. Temperatures were
0.5m1 of 100ppm phosphorous standard with the taken in-site. River and stream flows were laminar.
addition of 4m1 Murphy and Riley solutions and Twelve different quality parameters were analyzed
25m1-distilled water in a test tube. Blank solution for. Sites and site designations for water samples are
was prepared by measuring 4m1 ascorbic acid reagent given below:
and 25m1-distilled water into another test tube. The W1= water sample from River before quarry water
available soil phosphorous absorbance was read at a discharge point.
wavelength of 660 µm using the Corning Colorimeter W2= Sample from the point where quarry discharge
253. The phosphorus content was then calculated enters the river at a road bridge intersection.
(AOAC,1990). W3= Water sample from quarry pit floor.
W4= Quarry drainage water sample just before
Determination of Organic Matter entering the river.
Soil sample 1.0g was weighed and transferred into W5= Up-stream water sample of waste water receiving
250m1 conical flask. 10m1 of 0.5M potassium hepta- stream.
oxodichromate solution (K2Cr2O7) was pipetted into W6= Mid–stream sample of the stream containing
the flask and stirred properly to disperse the soil. factory effluent (along sugarcane plantation).
Concentrated sulphuric acid (H2S04) 20m1 was added W7= Sample from drainage combining drains form
to the solution and simultaneously swirled for proper raw mill, kiln control, cement mill, and dust
mixture and left to rest for a while. The flasks were recycling plant (DRP).
then gently rotated while shaking the contents and W8= Water sample from drainage connecting kiln
left for 30 minutes. Thereafter, 100m1 of distilled control and DRP drainages.
water was added to each solution, 4 drops of ferrion
indicator was also added into the mixture and titrated Water Analysis
against 0.25 molar ferrous sulphate solution. The end
pH
point showed light green turning into dark green and
with more gentle drops, the end point turned into pH values of water samples were measured using
brownish red. Burette readings were taken for each electronic pH meter. pH meter which had been
of the titrations. Standardization of dichromate was calibrated with two standard buffer solutions of pH
done by blank titration (i.e.) without the soil sample). 7 and pH 9(for an alkaline environment) was used
The organic matter content for each soil sample by inserting its electrode inside each water sample in
was calculated by multiplying the organic carbon turn( APHA, 1998).
percentage by a factor of 1.729 (AOAC,1990; Rao
and David, 2007). Turbidity:
Visual assessment by physical comparison of water
Exchangeable Cations determination (E.g. Mg2+,
samples with clean water was done.
Ca2+ Na+ and K+)
(Soil extraction (leaching) was followed by flame Determination of Conductivity
Emission photometry) The water conductivities of obtained water
Air-dried soil samples(< 2-mm) each weighing10.0g samples were determined using calibrated electrical
was added to 100m1 of ammonium acetate (NH4OAC) conductivity meter. The probe of the device was
solution. The mixtures were stirred with mechanical dipped in turn inside water samples and readings
shaker and allowed to rest for 1 hour and then filtered were taken (APHA, 1998).
by (110mm) filter paper. The filtrates were made up
to 200m1 and analyzed for exchangeable cation using
flame emission photometer at 767-nm wavelength. Determination of Fe2+ Pb2+ Ca2+ Al3+, Cr3+
However Atomic Absorption Spectrophotometer was Each water sample was decanted and filtered
used to determine Mg2+. through a new 0.45 μm pore diameter cellulose
18 ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011
acetate (membrane) filter. The filtrates were drops of phenolphthalein indicator was added to the
then placed directly in pre-sample filtrate cleaned sample and titrated against sulphuric acid until the pink
sample bottles. After filtration, 10% nitric acid colour disappeared. The result is ‘P’ phenolphthalein
(concentrated HNO3) pH <2 was added to filtrate in alkalinity i.e.OH-. To the colorless solution from
the bottles to stabilize/preserve the unstable metals. above, 1-2 drops of methyl orange indicator was
The water cation concentrations were determined added, the titration continued until methyl orange
using the Atomic Absorption spectrophotometer end point was reached. The final readings were taken
(APHA, 1998). and alkalinity calculated (APHA, 1998; Government
of India & Government of the Netherlands, 1999).
Determination of Biochemical Oxygen Demand
Determination of Hardness
The Biochemical Oxygen Demand (BOD) was
determined by measuring and recording the initial Water sample 50m1 was pipetted into 250m1 conical
dissolved oxygen (DOI) of each sample immediately flask. 3m1 of NaOH was added. 0.20–0.21 ammonium
after collection. The samples were then diluted with pupurate/solochrome black indicator was added. The
BOD free oxygen – saturated water and incubated (in solution was titrated against 0.01M ethylene-diamine
an air – tight controlled environment) with a 300m1– tatraacetic acid (EDTA), mixing it continuously
BOD bottle at 200C for 5 days. The final DOF was until the colour changed from pink to purple. EDTA
taken and recorded (APHA, 1998; Government of volume used was determined and total hardness as
India & Government of The Netherlands, 1999). CaCO3 mg/l was calculated (APHA, 1998).
Determination of Total Dissolved Solids(TDS)
RESULTS AND DISCUSSION
Water sample 100m1 was weighed and filtered
through whattman No 1 filter paper. Both suspended The various analyses conducted on soils, water
solids on filter paper and filtrates were dried on and dust samples obtained from the surrounding
evaporating dish at 1080C for 1 hour. The weight environment of the limestone and cement factory
difference between filtered paper and paper plus solid were aimed at examining the relationships between
was recorded as total suspended solids (TSS) in mg/l. the activities of the mine and its immediate
The weight difference between empty evaporating environment. In Table 1, the soil indicators which
dish and evaporating dish + sample was recorded and are major parameters for soil fertility and hence
the TDS (mg/l) calculated (APHA, 1998). vegetative growth (FAO,2005) are shown. Tables 3
and 5 show the various water samples analyses and
Determination of Alkalinity the composition of major oxides of the kiln dust
Water sample 100m1 was put into a beaker, 2–3 respectively.

SOIL

TABLE 1: Soil Analysis Result

ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011 19

 TABLE 2: General Rating / Classification of Soil Macro -nutrients, Micro-nutrients and Soil pH

NS= Not supplied

Source: FAO (1990) Soil Bulletin No 63, In: Federal Ministry of Agriculture, Water Resources
and Rural Development Publication.

FIG. 3: Soil organic matter and nitrogen

Soil organic matter is a constituent of the topsoil of low to medium based on Table 2. Soil sample S2
and the primary store house for most plant nutrients obtained from the virgin (Undisturbed portion of the
(macro and micro). It controls many chemical, physical mine) is classified low in organic matter; meaning that
and biological properties that affect the capacity of the specific area where this sample was obtained is not
a soil to produce food, fibres and fuel. It is the main as rich in organic matter. In Fig.3, soil samples S1 and
source of ecosystem energy, and also the main source S5 had the least percentages of organic matter and this
and a temporary sink of nutrients for plants in the agro- is a reflection of the deficiency of plants or vegetation
systems (Feller, 1995a). From Table 1, organic matter (main source of soil organic matter) on both the newly
ranged from (0.24-2.89) %; this indicates a soil rating reclaimed site and the dust dump site.

FIG. 4: Concentrations of macro and micro nutrients in soils

The analysis of soil macro nutrients(primary and could be attributed directly to the mine operations
secondary) revealed that some obtained values while others had no established relationship with
20 ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011
the operations. The primary macro-nutrients, N, P Cmol/kg with the least being sample S1(4.70)Cmol/
and K ranged from (0.01-0.15)%, (1.12-2.05)mg/ kg obtained from the dust dump site. This high
kg and (0.01-1.03)Cmol/kg respectively, while those concentration reflects the predominance of calcium
of secondary macro-nutrients, Ca and Mg varied in the limestone (CaCO3) mineral being mined in
between (4.70-9.60)Cmol/kg and (3.00-6.00)Cmol/kg the company. An excess of calcium in soil causes
respectively. magnesium, phosphate and trace nutrient deficiencies
Nitrogen in soils is the most important nutrient element (Ryan and Matar, 1992). Also, Phosphorous as an
in agriculture. However, higher concentrations of N anion is very reactive, and often tied up in the soil with
ion in the soil limit the uptake of other essential macro calcium and other cations. These calcium-phosphate
and micronutrients by plants(Vijay et al, 2009). The bonds are often very hard to break, especially in
obtained values of nitrogen across all samples including biologically weak soils, leaving the plant deficient
that of the undisturbed land S2 are rated medium to low (Joel, 1998).
(Table 2), hence no evidence of extraneous nitrogenous The alkaline nature of the calcareous soils in the
enrichment of the tested soils arising from mining limestone mine is again accentuated by the general high
activities or the cement processing. pH levels of the tested soil samples. Soil pH influences
Conversely, the concentrations of available nutrient levels as well because many macro- and micro-
calcium(Ca+) in all analyzed soil samples are nutrients are most accessible by plants within specific
comparatively high (Fig.4) ranging from (4.70-9.60) pH ranges (Schuster and Diemann, 2003).

WATER

TABLE 3: Results of Water Quality Analysis

VA = Visual Assessment
Turbidity Classification: NT =not turbid; ST = slightly turbid and VT = very turbid
ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011 21
 Water serves as an essential and integral part of the concentrations of both hardness and alkalinity
wet method of cement production from limestone. were highest in the water samples collected from mid-
Limestone -a sedimentary rock has in its matrix; stream of receiving stream where factory effluents is
interconnecting pore spaces making it a source rock discharged. Sample from the drainage connecting
for accumulation and discharge of water. The water drains form raw mill, kiln control, cement mill, and
used for the mines operation comes from water dust recycling plant (DRP) had the highest values
accumulated in the pit sump. Table 3 shows that only of Fe2+ concentration(6.2ppm) and total dissolved
sample (W1) with pH6.3 obtained from the upstream solids(TDS) of 250mg/l respectively.
side of the Odan river has a pH lower than pH 7. This Although in-situ turbidity measurement could not
buttresses the fact that the entire mine environment be carried out, it was visually observed that samples
is slightly alkaline in nature considering the pH values (W6, W7 and W8) all from post-factory drainage water
(6.3-7.5) obtained from all analyzed water samples. sources were very turbid in appearance having lots of
Most parameters had values within WHO and FEPA dispersed colloidal particles in them. Results show
standard limits for most samples. Values obtained for also revealed that metal-ion concentrations were
sample water (W1) which in this case was considered in all higher than the reference WHO standard for
as control showed that its hardness and CaCO2 potable water with the exception of aluminum which
alkalinity are 100mg/l and 140mg/l respectively. When had (0.00 - 0.2ppm) range in agreement with standard
compared with other samples, research revealed that limit.
22 ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011
 TABLE 4: Hourly Average of Electrostatic Precipitator (ESP) - trapped and Recycled Dust from Kilns 1 and 2 over a
period of Five Days

TABLE 5: Percentage Composition of Major oxides of Kiln Dust (Hourly Basis for 3 Hours)

LOI: Loss on Ignition

Tables 4 and 5 present dust generated from slurry- CONLUSION

roasting process by the factory two kilns and the
The research has examined some areas where
percentage compositions of major oxides of the kiln
direct mining activities and processing of limestone
dust respectively. From the data on Table 4, dust
could impact on the immediate environment of the
generation from the combined kilns 1 and 2 is estimated
mine. However, it is pertinent to note that whereas
at 28.22tonnes on an average hourly basis and at least
a very reasonable measure of data was collected
650tonnes per day. It is of note that failure in the
and subsequently analyzed, further research work
efficient operation of either or both kilns’ electrostatic
is still required to further extend the scope of work
precipitators (inbuilt mechanism for trapping dust)
to sections of the mine or factory which were not
would cause sizeable dust emission from their stacks.
touched such as soil test on old reclaimed land, dust
When this happens dust escapes into the air polluting
generation by vehicles at the mine face and dust from
the atmosphere. This is sometimes aided by wind
the cement mill.
action which often drives it to far distances; some
From the analyzed results, research has confirmed
lighter dust particles remain substantially airborne
that newly reclaimed land requires systematic
while the weightier ones settle down over some time.
approach in refilling the mined-out space with soil
When the weightier ones finally settle down, they
materials. Topsoil with humus layer having organic
destroy structural surfaces such as wall paints and
matter should be allowed to come last when backfilling
zinc panels of roof tops of nearby buildings and also
the voids with overburden materials. This will enhance
plug the stomata of plants leaves thereby inhibiting
quick vegetative growth. Similarly, the dust dump
their effective photosynthesis.
should be made flat instead of being conical and hilly
The silica content of the kiln dust averages 12.81
and possibly be wetted with crusting agents to prevent
%( Table 5). Silica content of dust is known to be
scavenging by wind.
responsible for occupational health disease called
The water from the raw mill and slurry de-silting
silicosis and mining continues to have some of the
pit showed elevated values of Fe2+ and Cr3+ as
highest incidences of work-related silicosis (NIOSH,
well high turbidity level. Hence, further investigation
2010). Failure to effectively control and contain the
is required to ascertain the root cause and proffer
kiln-generated dust could pose serious health hazards
technical solutions to them.
to cement factory workers; with some experiencing
short-term (acute) or long-term (chronic) dust-related
health problems.
ΟΡΥΚΤΟΣ ΠΛΟΥΤΟΣ/MINERAL WEALTH 157/2011 23
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