Beneficiation Flow Sheet Development of coal deposit from froth flotation

and dense media separation method of coal deposit in Gamo and Welaita coal
deposit in South Ethiopia.

By
Dagnaw yimer
A Project proposal Submitted to Center for Ethio-mines development
In Partial Fulfillment the requirement for the Degree of Masters of Engineering in
Mineral Process Engineering
Center for Ethio-mines development

Addis Ababa University Institute of technology

Jan 2023

Addis Ababa Ethiopia

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Table of Contents
Abstract.......................................................................................................................................................v
Chapter One..............................................................................................................................................1
1. Introduction.............................................................................................................................................1
1.1. Background of the study..................................................................................................................1
1.2. Statement of the problem...............................................................................................................2
1.3. Objective of the study......................................................................................................................2
1.3.1. General objective.....................................................................................................................2
1.3.2. Specific objective of the study.................................................................................................2
1.4. Scope of the study...........................................................................................................................3
1.5. Limitation of the study.....................................................................................................................3
1.6. Significance of the study..................................................................................................................3
Chapter Two..............................................................................................................................................4
2. Literature review.....................................................................................................................................4
2.1. Coal definition and its history..........................................................................................................4
2.1.1. Formation of coal.....................................................................................................................4
2.1.2. Classification of coal.................................................................................................................6
2.2. Coal mining......................................................................................................................................7
2.2.1. Surface mining.........................................................................................................................7
2.2.2. Underground mining................................................................................................................7
2.3. Coal production...............................................................................................................................8
2.4. Coal occurrence...............................................................................................................................9
2.5. Resource Classification and Reserve Estimation............................................................................10
2.6. Application of coal.........................................................................................................................10
2.6.2. in chemical industry...............................................................................................................10
2.6.3. in steel industry......................................................................................................................11
2.6.4. in cement industry.................................................................................................................11
2.7. Beneficiation techniques of coal....................................................................................................12
Chapter Three..........................................................................................................................................13
3. Materials and Methods.........................................................................................................................13

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 3.1. Apparatus and instruments........................................................................................................13
3.2. Chemicals and reagents..............................................................................................................13
3.3. Methods.....................................................................................................................................14
3.4. Sampling Techniques..................................................................................................................14
3.5. Experimental Design...................................................................................................................14
3.6. Sample Preparation and Particle Size Analysis............................................................................15
3.7. Proximate Analysis......................................................................................................................15
3.7.1. Moisture Content Determination.........................................................................................15
3.7.2. Volatile Matter Determination.............................................................................................16
3.7.3. Ash Content Determination..................................................................................................16
3.7.4. Fixed Carbon Determination................................................................................................16
3.8. Ultimate Analysis........................................................................................................................16
3.8.1. Determination of Nitrogen content by Kjeldahl Digestion...................................................17
3.8.2. Determination of Sulphur with Eschka Methods..................................................................17
3.8.3. Oxygen Content....................................................................................................................18
3.8.4. Determination of Calorific Value..........................................................................................18
Chapter 4. Research work plan schedule...................................................................................................19
Chapter 5. Budget Allocation....................................................................................................................21
Reference...................................................................................................................................................22

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Table of table

Table 1: Classification of coal grades based on ASTM-D-388.......................................................6

Table 2: coal composition on its type..............................................................................................8
Table 3: work plan schedule..........................................................................................................20
Table 4: Budget Allocation............................................................................................................21

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Table of figure
Figure 1: Formation of coal.............................................................................................................6
Figure 2: coal composition on its type.............................................................................................8
Figure 3: Co-production Potential flow sheet from Coal................................................................9
Figure 4: Coal Gasification flow chart..........................................................................................12

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Abstract
Coal is a combustible black or brownish-black sedimentary rock formed as strata, and dark
brown bands of coal deposits visible within the strata. Coal is mainly composed of carbon with
various amounts of other elements such as hydrogen, sulfur, oxygen and nitrogen. In Ethiopia,
coal is often considered to be of low quality because it contains a lot of ash, low levels of fixed
carbon, and low caloric value. The study will be conducted to improve the quality of coal by
reducing the amount of impurities in the coal particles and developing a beneficiation flow sheet
for a coal deposit. Experimental optimization of working conditions, float test, proximate
analysis value, ultimate analysis value, and ash content value and calorific value will be
performed with in froth flotation and dance media separation methods, and moisture content will
be determined by dry methods, than after development flow sheet.

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Chapter One
1. Introduction
1.1. Background of the study
Coal is a chemically and physically heterogeneous combustible sedimentary rock composed of
organic and inorganic matter. It is an organic rock enriched mainly in carbon with a low
concentration of hydrogen, oxygen, sulfur and nitrogen and few inorganic components, minerals
and water. It is a solid carbonaceous material usually brown or black most commonly found in
stratified sedimentary deposit. During and after the deposition of the plant remains
in the sedimentary basins, the organic remains undergo a series of physical, biochemical and
chemical changes (diagenesis and catagenesis) which result in a series of carbonizations.  The
series begins with unweathered plant material and peat and continues in ascending order of
precedence with lignite, sub bituminous, bituminous coal and finally anthracite. The
transformation of vegetable matter into peat and then into charcoal is considered to be
the biochemical or physico-chemical stage of carbonization (Behera et al., 2018).

To upgraded by using different technology of highly impure coal to minimizing the impurities
and to fit with its application. The recent techniques that are used for upgrading low-grade coal
are physical, chemical and physicochemical beneficiations (Hangil Park et al., 2021). These
techniques are used to increase the utility and cost-effectiveness of high ash and high sulfur-
containing coal. Physical and chemical beneficiation techniques are more selective for the
minerals separation and they are high economic cost with low efficiency. Besides the cost,
chemical reagents that are used in these techniques of coal purification are expensive and
dangerous that needs to be purified before discharging (Qianting Hu et al., 2015). The most
popular and significant technique in recent technology for beneficiation of low-grade coal is
physicochemical beneficiation. Physicochemical beneficiation is the most cost-effective and less
expensive separation of finely dispersed minerals to remove the inert materials based on the
hydrophobicity of coal particles and hydro philicity of mineral matters. Froth floatation is highly
economic and efficient techniques of physicochemical coal beneficiation methods. The basic
principles of froth floatation is based on surface wett ability of the fine coal and its separation
efficiency is based on attachment of the pure coal on the surface of hydrophobic oil reagents and
detachment of impurities matters from the surfaces (Park et al., 2021).

1
Therefore, the study will be aimed to purify the Gamo and Welaita coal deposits by using froth
floatation techniques of physicochemical beneficiation to separate impurity (minerals matter)
from pure coals, by improving the carbon content and calorific values and develop flow sheet. In
which purification of coal with physiochemical beneficiation through froth floatation is not
practiced in any Ethiopian industry (a O.-H.H et al.,2014).

1.2. Statement of the problem

The availability of coal in the country is high; its quality is very poor due to its high ash and
sulfur content. Hence the quantities of solid carbon of this coal and the calorific value are very
low. This impurity causes more damage to the equipment by causing corrosion and causes more
environmental pollution by releasing pollutants into the indoor air (Singh et al., 2016). Thus in
Ethiopia the demand for energy is out of balance with the supply, due to the expansion of
industrial zones and the improvement of living standards. This limitation of energy resources is
manifested in all parts of the country, cities, countryside and towns.

Therefore the local industries like cement and metallurgical steel industries are forced to use an
imported coal mainly from South Africa with the highest cost of foreign exchange (USD). To fill
this gap of high demand-supply and to substitute the imported coal, upgrading coal using
physicochemical beneficiation and flow sheet development is the solution to use the locally
available coal.

1.3. Objective of the study

1.3.1. General objective

The general objective of this project is to undergo flow sheet development for beneficiation
from froth flotation and dense media separation method of coal deposit in Gamo and
Welaita coal deposition in South Ethiopia.

1.3.2. Specific objective of the study

 Characterize the physiochemical proximate and ultimate analysis of Gamo and Welaita
coal deposit.
 Quantify the calorific value of the Gamo and Welaita coal deposit.
 Identifying the grade of the coal present in the study area.

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1.4. Scope of the study
The scope of this study is based on Gamo and Welaita coal deposit beneficiation flow sheet
development from froth flotation and dense media separation method. To implement the interest
of the ministry of mines that propos for 10th year’s project to produce quality coal based on the
agreement between with the center for Ethio-mines development located in Addis Ababa
University institute of technology.

1.5. Limitation of the study

The limitation of flow sheet development for the beneficiation of coal deposit in the given area from
froth flotation and dense media separation method is very time consuming and laborious to draw with
proper symbols and spacing. Excavating samples from study areas can be difficult and there may
also be a shortage of laboratories instruments to conduct them.

1.6. Significance of the study

The development of beneficiation flow sheet of Welaita and Gamo coal deposit from the froth
flotation and dense media separation method are the aim of the present study. Process conditions
affecting the separation features on air table will be identified and detailed individual effects and
interaction among the process factors will be quantified. The development of beneficiation flow
sheet of coal deposit is a step-wise representation of each activity in the coal beneficiation
process with in optimal condition and an excellent way of communicating with the interest group
about coal quality in this project. Developing flow sheet in the coal deposit beneficiation can be
analyzed and interpreted the problems more efficiently and effectively. Many different investors
and researchers could be used this project as an input secondary data for their activity. The study
is important for different readers to understand and obtain data on coal in the study area from
developed flow sheet.

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Chapter Two
2. Literature review
Coal is an organic fossil fuel and sedimentary rock that contains varying extents of carbon,
oxygen, hydrogen, sulfur and nitrogen as well as trace amounts of additional elements like,
mineral matter and methane which is found in the pore systems of the coal. It is a solid, brittle,
combustible, carbonaceous rock formed by decomposition and alteration of vegetation by
compaction, temperature, and pressure. The name of coal is assumed to be derived from the old
English name of “col” its kinds of charcoal at the time and it has a different name in a different
place. For example, in the northeast area of England, it was called “sea-coal” due to its
occasionally founded from washed up on beaches. In Ethiopian local peoples give different
names for coal such as “Dengay Kassel” in Amharic and “Dhaka cile” in Oromiffa (ABDI,
2021).

2.1. Coal definition and its history

Coal is an aggregate of heterogeneous substances composed of organic and inorganic materials.
The organic materials are derived mainly from plant remains which have undergone various
degrees of decomposition in the peat swaps and physical and chemical alteration after burial. The
bulk of all coal deposits were formed in a peat swamp environment where different types of
vegetation flourished, reflecting primarily condition of climate, water level and water chemistry
of the swamp (A.Meyers et al., 1982).

2.1.1. Formation of coal

The coal-forming process is simply defined as the progressive change of plant debris from the
peat to lignite and then through the higher ranks of coal to anthracite. So the formation of coal
was started during the period carboniferous which was called the first coal age and major coal
deposits were formed. This formation process of coal is through biological and geological
processes applying pressure and heat to peat over millions of years, which remains plant died, is
transformed into different rocks. In peat swamps formation the dead plant matter accumulates
cellulose rapidly oxidized by aerobic bacteria and other components produced are carbon dioxide
(CO2), methane (CH4) and ammonia from nitrogen-containing components. These aerobic
bacteria are quickly used up the available oxygen and then died at the last first stage of the

4
process at medium sufficient (pH =∼4) and produce acids as metabolic waste products (Hughes
et al., 2019).

Under anaerobic conditions the decay of dead materials which so-called biochemical stage of the
coal formation is a gel-like material that is termed Gytta (referred to as proto-coal). Then they
formed Gytta is buried to the depth of 500–1000 ft. with an application of temperatures
approximately 212 (100) in which moisture and volatile components are driven off to form
carbon-rich materials called peat. The proto-coal is undergone physical and chemical changes
during phase forming of rank formation are deposition and sedimentation, compaction, and then
transformation of the plant and fossil remains are changed into organic rocks. The geological
change is taking place over a long period by applying heat and pressure act on it to convert
deposits of organic rocks into today’s coal. The deposits of coal depend on pressure and heat
acting on the plant debris as it sank deeper and deeper over millions of years and provide the
energy that will be based on its deposited depth. The phase that occurs during coal formation are;
peat, lignite, bituminous and anthracite. These phases are depending upon the conditions to
which the plant and fossil remains are subjected after they are hidden the greater pressure and
heat, to change from lower ranks of coal to higher (Delhi et al., 2015).

Peat is the first stage in the formation of coal. Normally at this stage, the decays of dead
vegetable plants matters are oxidized into water and carbon dioxide. However, if plant material
accumulates underwater in the absence of oxygen only partial decomposition of the organic
substance occurs. So peat contains a large amount of water and a very low amount of carbon
number with more impurity and sufficient volatile matter (Mooney et al., 2010). Lignite is the
second process in coal formation, which is formed when peat is subjected to increased vertical
pressure from accumulating sediments. Like peat, it contains traces of plants that are not
completely decomposed. But its quality is very low because of more ash and sulfur content, due
to this; it is not intended for application before cleaning. Therefore it is characterized as low-
grade coal with low carbon content and limited to power generation; because of high ash and
sulfur, it produces more indoor air pollution with very high risks for environments. The third and
fourth phases of coal formation are bituminous and anthracite coal in which pressure is added to
this phase to make it more compact and virtually all traces of plant life have been disappeared.
So they are characterized with higher-ranking coal by having less moisture, volatile matters, and

5
low ash content, high carbon number with more heat value and less incombustible gases
(Shearer, 2002).

Figure 1. Formation of coal

2.1.2. Classification of coal

Coal classification is the ranking of different coal based on their qualities. According to the
ASTM-D-388 standards and degree of metamorphism with the elemental composition of carbon,
hydrogen, oxygen, nitrogen, sulfur and the amount of heat energy liberated coal can be classified
into four main types. Then the coal is categorized as lignite, sub-bituminous, bituminous and
anthracite.

Table 1: Classification of coal grades based on ASTM-D-388.

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2.2. Coal mining
Coal mining is generally classified as either surface or open cast mining and underground or
deep mining. Generally the type of coal mining selected is determined by the geological
characteristics of the proposed mine the location of the coal seam or seams and the equipment
available at the time the mine is to begin operation. Most coal is currently mined with one or
more underground methods to access the coal, which has been required given the machines
available when the mining will be started. However, with the introduction of larger and more
productive machines, surface mining is rapidly becoming the preferred method for both
productivity and safety (WESTVILLE et al., 2019).

2.2.1. Surface mining

Surface mining is used when the economics of removal of overburden to access the coal deposit
is viable. Generally, the coal must be fairly close to the surface but as machines increase their
capacity to move material, fairly close is becoming deeper and deeper. There are also several
categories of surface mining depending on the mining area. The most common is open cut where
the overburden is removed with draglines large electric shovels and bucket wheel excavators,
after it has been drilled and blasted. The overburden is usually loaded into large trucks and
removed to a waste area in the mine. The coal is then stripped usually after blasting, using
hydraulic excavators or loaders and removed from the mine using haulage trucks or conveyors.
Other types of surface mining include mountain top removal which is an alternative to doing
drift and/or slope mining. In some cases the entire top of a mountain might be considered
overburden and often removed to be used to fill in depressions nearby. Other rarer surface
methods include auger mining, where a trench is excavated and augers are used to extract the
coal usually in a narrow (thinner) seam and often from high wall mining where thicker seams are
sheared or excavated with special machinery (J. V. Bonta et al., 2007).

2.2.2. Underground mining

Underground mining in turn is classified according to how access to the coal is accomplished.
Thus an underground mine can be a drift mine where access is bored horizontally from the
surface to the deposit such as the side of a mountain; a slope mine where the shaft angles
downward, usually following the downward slope of the deposit; and where a shaft is sunk
vertically from the surface to the level or levels underground where the coal seam(s) can be

7
accessed. Underground mining usually falls into two operational categories: room and pillar in
which rooms of the coal deposit are mined usually with continuous miners leaving pillars or
blocks of coal to support the roof; and long wall in which the coal bed is blocked out into a panel
and a shearer machine cuts out the face of the coal seam. As the face is mined, hydraulic
supports hold up the roof of the mine after the shearer advances. The support is eventually
moved forward towards the newly exposed coal face allowing the roof to collapse in the so-
called goafvoid behind the working face. Room and pillar mining involves a sequence of
activities that are performed to first enter and develop the mine and then progressively extract the
coal. The continuous miner extracts the coal as it moves forward, loading it onto an attached
loader/shuttle car which in turn transfers the coal to a conveyor system. About every five meters
of advance, the miner is retracted from the face and moved to another ‘room’. It is replaced by a
‘rock-bolting’ machine that drills into the roof and sometimes the walls, and places ‘bolts’ (often
made from fibrous material) to secure and bond the strata to prevent caving.

Table 2: coal composition on its type

2.3. Coal production

The largest coal producing countries are not confined to one region. The top five producers are
China, USA, India, Australia and South Africa. Much of global coal production is used in the
country in which it was produced; only around 16% of hard coal production is destined for the
international coal market. According to world energy council global coal production is expected
to reach 7000 MT in 2030 with China accounting for around half the increase over this period.
Steam coal production is projected to have reached around 5200 MT, coking coal 620 MT, and
brown coal 1200 MT (DEMOZE, 2007).

8
 Figure 3: Co-production Potential flow sheet from Coal.

Coal Gas: Coal gas is Coal gas is a mixture of hydrogen (40%), methane (32%), carbon
monoxide (7%), acetylene (2%), ethylene (3%), nitrogen (4%), carbon dioxide (1%) and some
other gases (4%). It is originally developed as a by-product of the coking process before the
industrial revolution. The use of coal to manufacture gas for fuel was prominent in the 1940s and
1950s prior to the development of natural gas. The development of the natural gas industry led to
the decline in the demand and popularity of the use of coal gas. Natural gas has an energy
content of 37 MJ/m3 compared to the 10-20 MJ/m3 of coal gas (Ndlovu et al., 2020).

2.4. Coal occurrence

Ethiopia is endowed with several natural resources like natural gas, geothermal, coal and many
other resources. The occurrence of coal in Ethiopia belongs to the Cenozoic age and it is
associated with the lacustrine sedimentary rock. This occurrence of coal is distributed in some
parts of the country that assures more coal reserves which serve as a bridge for building

9
industrial development and sustainable agriculture use of coal reserves. The exploration of coal
deposits is an integral part of searching for energy resources. The occurrences and distribution of
coal in different areas of Ethiopia such as; Gamo, Wellayita, Delbi-Moye, Jiren, Yayu (Geba
basin), Lalo-Sapo, Chida, Chilga, Nejo, Arjo, Wuchale and Mush valley Basins (RAASK, 1985).

2.5. Resource Classification and Reserve Estimation

Coal resources categories range from the general evaluation of a coal basin to the calculation of
specific reserves located within mine workings. The final result of geological investigation of a
coal deposit will be to calculate all categories of coal resources. Different countries have their
standard for the classification of coal resource and reserve. But, a committee of the Council of
Mining and Metallurgical Institutions of different countries use a provisional agreement for the
use of standard definitions and method of calculation for mineral resources (inferred, indicated
and measured) and ore reserves (probable, proven and marketable) which is approved by
Combined Reserves International Reporting Standards Committee (mihretie et et., 2018). The
basic formula to calculate coal resources is (for each defined resource/reserve block): Coal
thickness (m) × area × RD = total metric tons, Where, RD stands for relative density.

2.6. Application of coal

Coal has many important applications throughout the world; the most significant uses of coal are
for electricity generation, steel production, cementing manufacturing and as a source of energy
for household and uses as feedstock in the different chemical industry. Several chemical products
can be produced from a by-product of refined coal tar to produce phenol, benzene and
naphthalene by converting coal into gases by gasification processes (Abraham, 2018).

2.6.1. in chemical industry

The most common and first stage using coal as feedstock in industries is gasification of coal in
which coal is undergoing pyrolysis at high temperature to change into gases. This gasification is
used to produce synthesis gas (CO & H2) which serves as starting materials for other chemical
products.

Besides heat source coal is used as raw materials in a variety of industries like limestone, bricks
and chemical products (Figure 5). The separated ingredients of the coal (like methanol and

10
ethylene) are used for making plastics, tar, synthetic fibers, propylene gas, Hydrocarbons and
ammonia/fertilizers.

Figure 4: Coal Gasification flow chart

2.6.2. in steel industry

Steel is an alloy based primarily iron which is occurred in the forms of iron oxides in the earth’s
crust. In the steel industry, coal is used indirectly to make steels whereby coal is baked in blast
furnaces to form coal cake, which is used to smelt iron ores into iron for making steels. Coking
coal is vital for sustainable steel manufacturing, with over 70% of universal production of steel
from iron ore. The iron ores must be converted or reduced by using coal, which is a primary
source of carbon which is obtained from coal. The purpose of coal baked at high temperature to
give strength and flexibility to steel products that are used in bridges, buildings, and automobile
making. Meanwhile, the ammonia gas is usually recovered from coke ovens, which are used to
manufacture nitric acid, ammonia salts and fertilizers (Wakuma et al., 2017).

2.6.3. in cement industry

Coal is used as an energy source in the cement industry, which is the essential commodity in the
construction industry of bridges, buildings, dams, roads and airports. Cement is made from a
mixture of silica, calcium carbonate, alumina and iron oxide at high-temperature in the kiln to
melt this raw material. The coal is used in the cement industry in two stages, first in a precalciner
stage that uses to produce calcium oxide and carbon dioxides from calcium carbonate by using

11
greater than 4000 kcal heat value of coal. The second stage of coal usage is in a kiln (main
burner) to produce clinker by using fine coal greater than the calorific value of 5000 kcal (1400-
1450oc). For example, producing one ton of cement requires about 200 kg of fine coal (Vienna,
2016).

2.7. Beneficiation techniques of coal

Froth flotation process utilizes the differences in Physico chemical surface properties of various
minerals. The treatment of the ore pulp with the reagents creates favorable conditions for the
attachment of certain mineral particles to air bubbles. The air bubbles carry the selected minerals
to the surface of the pulp and from a stabilized froth which is skimmed off while the other
minerals remain in the suspension. Bench scale flotation studies were performed in Dorr - Olvier
laboratory cell type with a capacity of 6L. Flotation studies have been carried out with the
combine 0.5 mm size fraction at optimized conditions (Maij et al., 2018).

12
Chapter Three
3. Materials and Methods
Flow sheet development for beneficiation of coal deposit in Gamo and Welaita in South Ethiopia
to overcome this project objective different method will be following. They are mainly divided
into three phases; pre-field work, field work and post-field work activities. During each different
phases, a variety of tools will have used including; topographic (1:150,000) and geological maps
(1:250,000), standard field sampling and measuring equipment (such as GPS, Brunton compass,
Camera, geological hammer, meter, sample sack and 10× hand lens) and Arc GIS, surfur, DEM,
Global mapper and Google Earth software’s.

3.1. Apparatus and instruments

The apparatus and instruments used in this study are; Universal Hot Oven (Jaico fisher scientific
40GCEMD, India), Kjeldahl Digester (BUCHI K-439, Swizerland), Silica crucible, Desiccator,
Muffle furnace (XMT-F9), Electronic balance(AUW 320, philiphenes) at Addis Ababa Science
and Technology University (Industrial chemistry and Food science lab.), Jaw crusher
(RoHs53743, Germany) , Centrifugal mill (RETCH 56402, Germany), Sieve Shaker (RETCH
A200, Gemany), Wedag flotation cell (Groppel 98, west Germany) at Addis Ababa Institute of
Technology (Mechanical operation lab.), Adiabatic Bomb calorimeter (MK GSL-12, United
kingdom) at Geological Survey of Ethiopia (Central laboratory), Flash CHNS/O analyzer
(EA1112, Japan) at Addis Ababa University, Chemistry Department (Inorganic lab).

3.2. Chemicals and reagents

The chemical reagents which will have used for this study are; Diesel oil(Industrial grade), N-
Octanol (99% Loba chemie Ptv.Ltd, India), Sodium hydroxide (98% Sigma -Aldrich, USA),
Sulphuric acid (98% Sigma -Aldrich, USA), Boric acid(99.5% Loba chemie pvt.Ltd, India),
Hydrochloric acid(37%Sigma -Aldrich, USA), Kjeldahl tablets (0.15gm of CuSO4 & 1.5gm of
K2SO4) (98.5% BUCHI,Swizerland), Magnesium oxide (97.5% Sigma-Aldrim, Munich
Germany) Sodium carbonate anhydrous (99.9% Sisco Research Laboratiroies pvt.Ltd, India) ,
Tashoro’s indicators (MR& BCG).

13
3.3. Methods
Flow sheet development in coal deposit beneficiation methods is conducted at Gamo and
Welaita: based on the chemical and physical composition of collected a channel or core sample
of coal will have analyzed according to International and national standards coal analyses
guidelines that is American Society for Testing and Materials standards for coal analyses
(ASTM). In order to determine the quality of coal, two types of analysis are carried out:
Proximity analysis and Ultimate analysis. Proximity Analysis of coal gives an idea of gross
impurities present in its composition. This method is used to determine moisture content, volatile
matter, ash content and fixed carbon of coal based on American Society for Testing and
Materials (ASTM). It provides important information regarding the suitability of coal for a
particular domestic or industrial use.
The accessibility of the targeted area is found with asphalt main way that joins Addis Ababa to
Arbaminch road. This way is passing through the town such as ziway, hawassa, welaita, konso
then Gammo.

3.4. Sampling Techniques

The sample collection techniques from each sampling site are based on the International
standards of coal analyses guidelines (ASTM D-2234). During sampling, the conditions such as
recording the location area, the thickness of the seams, recording the depth and elevation site of
drilled holes must be taken into consideration. The equal representation of samples from all
layers of sampling sites is collected in plastic bags with an amount of 3 to 5 kg. From all three
sampling sites, in Gamo stream the coal will have seen arranged in their layers, due to this the
sampling is based on these layers. From three sampling sites, a total of 12 samples are collected
with a total mass of 45 kg by weight. Finally, the sample is transported from Gamo and welayita
to Addis Ababa University Institute of Technology.

3.5. Experimental Design

Overall experimental procedure will be performed in this study. This includes sampling and
preparation methods up to the final analytical stage with instrument characterization. This
experimental procedure is designed for both live and suspension samples.

14
3.6. Sample Preparation and Particle Size Analysis
The collected sample is prepared based on ASTM D-2013. This includes drying the sample in
air, crushing, dividing, and mixing the gross sample to obtain the sample ready for laboratory
analysis. In the first step, immediately after traveling to AAiT, the samples are dried in
atmospheric air for 72 hrs for removal of extraneous moisture of the coal sample. Then, the dried
coal sample is ready for size reduction by taking the required amounts of the sample from each
site. The main purpose of size reduction is to minimize the particle size without changing the
proportional weight. The lumpy coal sample is crushed to reduce the size of the particle to 1-2
mm by jaw crusher. Then to obtain the fine powders product approximately less than 500 μm
centrifugal millers is used. The milled particle will have taken to the sieve shaker to separate the
fine and coarse samples. The mesh sieve is arranged from higher to lower size (500-250 μm or
60 meshes, 250-125 μm or 120 meshes and 125-63 μm or 230 meshes. Finally, the fine powder
product of the Gamo and Welaita coal sample is stored in plastic bags and taken to the laboratory
for analysis.

3.7. Proximate Analysis

The proximate analysis is telling about the idea of gross impurity presences in the sample. This
method is used to determine the moisture content, volatile matter, ash content and fixed carbon
content (Usman et al., 2021)..

3.7.1. Moisture Content Determination

The determination of the total moisture was according to the standards ASTM D-3302, 2 g of the
air-dried fine coal sample was taken in silica crucible and gently heated in the hot oven with an
experimental temperature of 107 for three hours. The heated sample was taken from the hot oven
and put in a dissector to cool down, and then the cooled sample was reweighed. The process of
heating, cooling and weighing of the sample will have repeated twice and an average result is
reported (Usman et al., 2021).

loss∈weight
Percentage of moisture contente= ∗100 %
weight of sample taken

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3.7.2. Volatile Matter Determination
The percentage of the volatile matter is determined according to the testing method of ASTM D-
3175; 1 g of an air-dried sample will have weighed in a silica crucible and covered with a lid to avoid
oxidation of the sample. Then the sample is heated at a temperature of 950±5 in a muffle furnace
exactly for seven minutes in the absence of air. After heating and putting in dissector for cooling and
re-weighed again (Usman et al., 2021). The process will have repeated twice and the average result
will be reported.

loss∈weight
percentage of volatile matter= ∗100 %−moisture %
mass of sample taken

3.7.3. Ash Content Determination

The amount of ash is used to determine based on the standard procedure of ASTM D-3174. Then
1 g of the sample will have weighed in silica crucible and heated in a muffle furnace at 850±5 in
presence of air for 3 hours. After burning the residue of ash will have cooled in a dissector and
reweighed again. All process will be repeated twice and the average result will have reported
(Usman et al., 2021). Finally, the ash content will be calculated.
weight of ash residue
percentage of ash= ∗100 %
weight of dried coal sample

3.7.4. Fixed Carbon Determination

The percentage of fixed carbon of coal sample well be determined according to ASTM D-388
standards. Then fixed carbon is determined by subtracting the sum of moisture matter, volatile
matter and ash content (Usman et al., 2021).

percentage of ¿ carbon=100−¿+ash % ¿

3.8. Ultimate Analysis

The ultimate analysis tells that the elemental composition of the coal will be determined by using
EA 1112 flash CHNS/O analyzer. The working conditions of the analyzer are carrier gas flow
rate (120 ml/min), reference flow rate (100ml/min), oxygen flow rate (250 ml/min), furnace
temperature (900), oven temperature (75) and oxygen injection time (5 sec). A 3 mg of powder
samples are weighed in a tin container and then introduced into the combustion reactor through
the Thermo Scientific MAS plus Auto-sampler with the help of oxygen. After combustion, the

16
resulted gases are conveyed by helium flow to a layer filled with copper, then swept through a
GC column that provides the separation of the combustion gases (Usman et al., 2021). Finally,
Thermal Conductivity Detector (TCD) will be used for detecting the results.

3.8.1. Determination of Nitrogen content by Kjeldahl Digestion

5.00 g of coal sample is weighed and put into Kjeldahl digestion flask with 50 ml of sulfuric acid and
two Kjeldahl tablets are added as a catalyst to increase the boiling point of sulfuric acid and speed up
the efficiency of digestion. Then the flask will be slightly heated in an inclined position with the
adjusted working temperature at 390 and allowed to boil for 7 hours. During the digestion, the NH 4+
ion ((NH4)2SO4) is formed and the mixture is diluted with 250 ml of distilled water for cooling down.
To neutralize the solution and convert the NH 4+ ion into ammonia gas excess of 125ml (50 % (w/v))
of sodium hydroxide is added. Then the flask will have connected to the Kjeldahl distillation
apparatus and followed by boiling and condensation of gas with 70 ml (4 % (w/v)) of boric acid will
be added that followed by 6-9 drops of Tashoro’s (MR and BCG) indicator in the receiving flasks for
7 min. Finally, the distillate is titrated against 0.1 M hydrochloric acid. The same procedure is
repeated for the blank solution (Usman et al., 2021). Then the percentage nitrogen (% N) will be
calculated.

V 2 ( ml )−V 1 ( ml )∗0.1 M∗14.007 g /mol

Nitrogen∈%= ∗100 %
weight of sample taken

3.8.2. Determination of Sulphur with Eschka Methods

Sulfur in the coal sample is determined according to ASTM D-3177 standards. 1 g of coal
samples will be weighed in a porcelain crucible and mixed with 3 g of Eschka mixtures (2 g of
magnesium oxide and 1 g of anhydrous sodium carbonate). The mixture is covered with another
1 g of Eschka mixture for preventing the loss of sulfur as sulfur dioxide. Then the crucible will
be put in a cold muffle furnace and heated gradually at 800 temperatures for 60 minutes. The
compounds of Sulphur that evolved during combustion are reacted with Eschka mixture under
oxidized conditions; both are converted to Sodium Sulphate and Magnesium Sulphate. Then the
product is digested by dilute 1 M of HCl solution with intermittent stirring for 45 min. The
digested solution is filtered into 400 ml beakers and three drops of methyl orange are added until
the color is turned to neutral. Next, the sample will have heated to boiling and 10ml of BaCl2 (10
%) is gradually added while stirring in continuous boiling for 30minutes. Finally, the solution

17
will be filtered after cooling down by thoroughly washing with hot water and the residue BaSO4
is formed and burned at 500 and weighed (Kalenga, 2011). The formed BaSO4 will be used to
calculate the sulfur content in coal samples by using this Equation.

32 weight of BaSO 4 formed ( g )

Sulpher∈%= + ∗100
233 weight of sample taken ( g )

3.8.3. Oxygen Content

The percentage of oxygen content in the coal sample was calculated by subtracting the sum of
ultimate Carbon, Hydrogen, Nitrogen, Sulfur, Moisture matter and Ash content (Usman et al.,
2021).. % Oxygen = 100 − (Carbon + Hydrogen + Nitrogen + Sulphur + Ash)%

3.8.4. Determination of Calorific Value

The calorific value of the coal sample will be determined by using an adiabatic bomb calorimeter
through equivalent standards of ASTM D-2015 which shows between 25-35MJ/kg value standard.
Approximately 1 g of powder sample is weighed in nickel crucible and placed in a bomb. Then the
crucible is tied with 10 cm of fuse wire on two supporting rings and the bomb is covered by a lid.
Then the Oxygen supply is purged across the valve into the bomb until the pressure is reached 25-30
atm for completing the combustion and the bucket of the calorimeter is filled with 2000 ml of
distilled water. After the initial temperature and jacket temperature is equilibrated bucket temperature
is started to rising from its initial temperature. Then the maximum temperature is recorded and the
bomb is removed and the valve is open gradually to release the residual gas pressure before
attempting to remove the cap. The interior surfaces of the bomb are washed with distilled water and
collected in a beaker. All unburned pieces of fuse wire from the bomb electrode are removed and
measured to know the net amount of fuse wire burned. Finally, the bomb washing is titrated with a
standard sodium carbonate solution using a methyl orange indicator (Usman et al., 2021). Then the
gross heat combustion is calculated.

(tW −e 1−e 2−e 3)

GCV =
m

Where

GCV= Gross calorific value in Btu/lb.

t = the temperature change
W = energy equivalent of calorimeter in cal/oC

18
e1= correction in calories for heat of formation of nitric acid (HNO3)
e2= correction in calories for heat of formation of sulpheric acid
e3= correction in calories for heat of combustion fuse wire
m=mass of coal sample taken in grams

19
Chapter Four

4. Research work plan schedule

 Year of work plan 2023

No list of activities Dec Jan Feb Mar Apr Mey Jun

1 Title selection
2 collecting of resources,
literature review collecting of
resources, literature review
3 Defense of proposal

4 Sample collection: Physical,

chemical and mineralogical
characterization.
5 Crushing, grinding, and sieve
analysis.
6 Froth flotation

7 Dense media separation.

8 Ultimate, proximate and coal

quality analysis.
9 Data processing, interpretation
and conclusion
10 Project defense

Table 3: work plan schedule

20
Chapter Five
5. Budget Allocation
No Instrument ETB No day Tot ETB
1 Sample collection 5000 15
2 Jaw Crusher 5000 5
3 Universal Hot Oven 10,000 7
4 Kjeldahl Digester 10,000 7
5 Silica crucible 5000 2
6 Desiccator 5000 3
7 Muffle furnace (XMT-F9) 7000 2
8 Centrifugal mill (RETCH 6000 2 62,000
56402, Germany)
9 Sieve Shaker (RETCH A200, 3000 2
Gemany)
10 Adiabatic Bomb calorimeter 6000 5
(MK GSL-12, United
kingdom) at Geological Survey
of Ethiopia (Central laboratory)
Table 4: Budget Allocation

21
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