Addis Ababa University

School of Graduate Studies

Addis Ababa Institute of Technology
School of Chemical and Bio Engineering

Optimization of Gypsum Processing Parameters For the

Production of Improved Quality Chalk

By
Gemechu Bushu

A Thesis Submitted to the School of Graduate Studies of Addis Ababa

University, Institute of Technology, in Partial Fulfillment of the
Requirements for the Degree of Masters of Science in Chemical
Engineering (Process Engineering)

Advisor
Dr. Tassisa Kaba

December 17, 2014

Addis Ababa
Ethiopia
 Addis Ababa University
School of Graduate Studies
Addis Ababa Institute of Technology
School of Chemical and Bio Engineering
Optimization of Gypsum Processing Parameters For the
Production of Improved Quality Chalk

By
Gemechu Bushu

A Thesis Submitted to the School of Graduate Studies of Addis Ababa

University in Partial Fulfilment of the Degree of Master of Science in
School of Chemical and Bio Engineering (Process Engineering)

Approved by Board of Examiners

Name Signature Date

Chair man, Graduate Committee

Advisor

Internal Examiner

External Examiner
ACKNOWLEDGEMENT
Above all, I would like to thank the Almighty GOD for giving me the strength and wisdom
to successfully complete this thesis for his protection and a present helps in the entire
situation and challenge that I face. Moreover, I would like to express my heartfelt appre-
ciation and thank to my Instructor and now thesis research advisor Dr. Tassisa Kaba for
the opportunity he gave me to work with him, for his valuable advice, comments on my
work, his sustainable and appreciable guidance, tireless advising, for sharing his knowl-
edge, skill, experience and fine-tuning up to the successful completion of this thesis.

I am deeply indebted Ato Ferenge Kelbamo, Ato Wendimagegn and all my friends for
their invaluable advice in the preparation of this thesis and their encouragement. Fi-
nally, I am deeply grateful to my friend, Belaynesh Berihun, for her patience and love,
and to all members of my family for their devoted support and encouirement through-
out the period of my study.

Thanks also go to all the people I met during the thesis work for their invaluable con-
tributions to my work, whom I could not name them here due to limited space. Lastly
and certainly not in the least, many thanks go to all technician assistants, colleagues and
batch of 2005. Thank you all for sharing your knowledge and experience.This work is
dedicated to my parents for all the support and motivation they have given me through-
out my life.

i
TABLE OF CONTENTS
LIST OF ABBREVIATIONS v

LIST OF TABLES vi

LIST OF FIGURES vii

ABSTRACT viii

1 INTRODUCTION 1
1.1 Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.2 Statement of the Problem . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.3 Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.3.1 General Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.3.2 Specific Objectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.4 Significance of the Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2 LITERATURE REVIEW 4
2.1 The Structure of Gypsum System . . . . . . . . . . . . . . . . . . . . . . . . 4
2.2 Geological Occurrence and Abundance of Gypsum . . . . . . . . . . . . . . 4
2.3 Occurrence of Gypsum in Ethiopia . . . . . . . . . . . . . . . . . . . . . . . 5
2.4 Production of POP and Chalk in Ethiopia . . . . . . . . . . . . . . . . . . . . 6
2.4.1 Production of Plaster of Paris . . . . . . . . . . . . . . . . . . . . . . 6
2.4.2 Production of Chalk . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5 The Physico-Chemical properties of Gypsum . . . . . . . . . . . . . . . . . 8
2.6 Technology Selection and Production Process of POP . . . . . . . . . . . . 10
2.6.1 Size Reduction Process . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.6.2 Kettle Calcinating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.6.3 Plaster of Paris (POP) . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.7 Gypsum Dehydration Sequence . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.8 Technology Selection and Production Process of Chalk . . . . . . . . . . . . 15
2.9 Different Processing Parameters on Chalk . . . . . . . . . . . . . . . . . . . 18
2.10 Other Possible Raw Materials to Produce Chalk . . . . . . . . . . . . . . . . 19
2.11 Application of Gypsum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
2.12 Environmental Implications . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

3 MATERIALS AND METHODS 21

3.1 Time and Place of the Study . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.2 Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.3 Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.3.1 Source and Preparation of Raw Materials Sample . . . . . . . . . . . 21
3.3.2 Size Reduction of the Sample . . . . . . . . . . . . . . . . . . . . . . 22

ii
 3.3.3 Calcinations Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . 22
3.3.4 Mixing Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
3.3.5 Moulding Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . 23
3.3.6 Drying Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
3.4 Proximate Determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
3.4.1 Determination of Moisture Content . . . . . . . . . . . . . . . . . . 23
3.4.2 Determination of Bulk Density . . . . . . . . . . . . . . . . . . . . . 24
3.4.3 Determination of Breaking Strength . . . . . . . . . . . . . . . . . . 24
3.5 Experimental Design of Process Parameters . . . . . . . . . . . . . . . . . . 24
3.6 Factors Affecting the Quality of the Product . . . . . . . . . . . . . . . . . . 26
3.6.1 Experimental Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

4 RESULTS AND DISCUSSION 28

4.1 Characterization of the Raw Materials . . . . . . . . . . . . . . . . . . . . . 28
4.1.1 Physical Characterization . . . . . . . . . . . . . . . . . . . . . . . . 28
4.1.2 Chemical Characterization . . . . . . . . . . . . . . . . . . . . . . . 28
4.2 Statistical Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.2.1 Optimization using Desirability . . . . . . . . . . . . . . . . . . . . . 30
4.2.2 Development of Regression Model Equation . . . . . . . . . . . . . 32
4.3 Data Analysis of Process Parameters . . . . . . . . . . . . . . . . . . . . . . 33
4.3.1 Data Analysis for Bulk Density . . . . . . . . . . . . . . . . . . . . . . 34
4.3.2 Data Analysis for Breaking Strength . . . . . . . . . . . . . . . . . . . 35
4.3.3 Diagnostic test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
4.3.4 Effect of Processes Parameters on the Responses . . . . . . . . . . . 37
4.3.5 Optimization of the Process Parameters . . . . . . . . . . . . . . . . 42
4.3.6 Validation of Optimum Results . . . . . . . . . . . . . . . . . . . . . 43

5 FEASIBILITY STUDY OF IMPROVED QUALITY CHALK 45

5.1 Product Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.2 Quality Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
5.3 Material and Energy Balance . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5.3.1 Material Balance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5.3.2 Energy Balance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
5.4 Design of Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
5.5 Financial Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
5.5.1 Total Capital Investment . . . . . . . . . . . . . . . . . . . . . . . . . 54
5.5.2 Total Product Cost . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.5.3 Profitability Measurements . . . . . . . . . . . . . . . . . . . . . . . 57
5.6 Plant Location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58

iii
6 CONCLUSION AND RECOMMENDATION 59
6.1 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
6.2 Recommendation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

REFERENCES 61

APPENDICES 65

Appendix A: Experimental Design Run Sheet 65

Appendix B: Statistical Results Tables 65

Appendix C: Statistical Results Figures 65

iv
LIST OF ABBREVIATIONS

2FI Two Factor Interaction

3-D Three-dimensional
ANOVA Analysis of Variance
AI Anhydrite I
AII Anhydrite II
AIII Anhydrite III
CCD Central Composite Design
CI Confidence Interval
Cp Specific Heat Capacity
CT Calcinations Temperature
C.V Coefficient of Variation
D Dehydrate
Df Degree of Freedom
EMDPE Educational Material Production and Distribution Enterprise
FCCD Face Centered Composite Design
FGD Flue Gas Desulphurization
GSE Geological Surveys of Ethiopia
LSD Least Significant Difference
MC Moister Content
MS Mean Square
POP Plaster of Paris
PS Particle Size
RSM Response Surface Methodology
SS Sum of Squares
Std. Dev. Standard Deviation

v
LIST OF TABLES
1 Compositions Yogef gypsum occurrence[15] . . . . . . . . . . . . . . . . . . 6
2 Production of POP in Ethiopia in consecutive ten years . . . . . . . . . . . 7
3 Imports of Plaster of Paris . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
4 Production of Chalk in Ethiopia in consecutive five years . . . . . . . . . . 7
5 Quantity of Chalk Imported . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
6 Physical and chemical properties of gypsum . . . . . . . . . . . . . . . . . . 9
7 Comparison of alpha and beta plaster . . . . . . . . . . . . . . . . . . . . . 12
8 Phases of gypsums . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
9 Physical properties of gypsum, hemihydrate and anhydrite . . . . . . . . . 15
10 Hemihydrates, anhydrates, and respective calcining temperatures[36] . . . 15
11 Specification of chalk . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
12 Coded and Actual levels of the variables for CCD of the RSM . . . . . . . . 26
13 Experimental design setup using design expert CCD . . . . . . . . . . . . . 27
14 Physical characterization of the raw materials . . . . . . . . . . . . . . . . . 28
15 Compositional analysis of Kentry gypsum . . . . . . . . . . . . . . . . . . . 28
16 Compositional analysis of Kentry gypsum after crushed . . . . . . . . . . . 28
17 Compositional analysis of Filiklik gypsum . . . . . . . . . . . . . . . . . . . 29
18 Compositional analysis of lower and upper Yogef gypsum . . . . . . . . . . 29
19 Comparison of compositional analyses for the raw materials . . . . . . . . 29
20 Statistical results for actual and experimental . . . . . . . . . . . . . . . . . 31
21 Optimization criteria used in this study . . . . . . . . . . . . . . . . . . . . 32
22 Analysis of variance table for improved model for Bulk Density . . . . . . . 34
23 Analysis of variance table for improved model for Breaking Strength . . . . 35
24 Optimum solutions obtained depending on the desirability . . . . . . . . . 42
25 Validation test results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
26 The comparison of this result with the literature review . . . . . . . . . . . 43
27 Demand and supply of chalk in Ethiopia (2000 - 2013) . . . . . . . . . . . . 45
28 Purchased equipment cost . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
29 Fixed Capital Investment Cost . . . . . . . . . . . . . . . . . . . . . . . . . . 55
30 Raw and auxiliary materials, Utilities cost and Operating Labor Cost . . . . 56
31 Experimental Design Run Sheet . . . . . . . . . . . . . . . . . . . . . . . . . 65
32 Design Summary of Designs Expert . . . . . . . . . . . . . . . . . . . . . . 65
33 Regression Coefficient of 2FI and Significance for Bulk Density . . . . . . . 66
34 Regression Coefficient of quadratic and Significance for Breaking Strength 66

vi
LIST OF FIGURES
1 Schematic illustration of the layer structure of gypsum [7] . . . . . . . . . . 4
2 Section of the crystal structure of gypsum; the horizontal dotted line shows
the plane of cleavage through the water molecules[9] . . . . . . . . . . . . 5
3 Production Chalk in Ethiopia . . . . . . . . . . . . . . . . . . . . . . . . . . 8
4 The process flow diagram of POP production line[29] . . . . . . . . . . . . 11
5 Plaster production process . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
6 The process flow diagram of batch- type manual chalk production line[47] 17
7 The process flow diagram of automated continuous-type production line . 18
8 Flowchart Outlining the Analysis Steps Undertaken . . . . . . . . . . . . . 25
9 Plots of Residuals for a) bulk density b) breaking strength . . . . . . . . . . 36
10 Plot of the actual and predicted values for a) bulk density b) breaking strength 36
11 Cubic representation of interaction effects of the three factors on bulk den-
sity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
12 Response surface plots for bulk density as a function of three factors . . . . 39
13 Cubic representation of interaction effects of the three factors on breaking
strength . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
14 Response surface plots for breaking strength as a function of the three factors 41
15 Material balance for dryer . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
16 Material balance for moulder . . . . . . . . . . . . . . . . . . . . . . . . . . 48
17 Material balance for mixer . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
18 Material balance for Pulverizer . . . . . . . . . . . . . . . . . . . . . . . . . 49
19 Material balance for kettle . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
20 Material balance for grinding mill . . . . . . . . . . . . . . . . . . . . . . . . 50
21 Material balance for secondary crusher . . . . . . . . . . . . . . . . . . . . 51
22 Material balance for jaw crusher . . . . . . . . . . . . . . . . . . . . . . . . . 51
23 Energy Balance on Kettle Calciner . . . . . . . . . . . . . . . . . . . . . . . . 52
24 Energy Balance on Dryer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
25 Perturbation plots for (i) bulk density and (ii) breaking strength . . . . . . 66
26 Direct effect of the three factors on the bulk density . . . . . . . . . . . . . 66
27 Direct effect of the three factors on the breaking strength . . . . . . . . . . 67
28 Effect of two factor interactions on bulk density . . . . . . . . . . . . . . . 67
29 Effect of two factor interactions on breaking strength . . . . . . . . . . . . 67
30 Contour plots for bulk density . . . . . . . . . . . . . . . . . . . . . . . . . . 68
31 Contour plots for breaking strength . . . . . . . . . . . . . . . . . . . . . . 68

vii
ABSTRACT
The study was conducted with objective that find the optimum value of the gypsum pro-
cessing parameters for the production of improved quality chalk using locally available
raw materials. Gypsum rocks with size less than 20cm in diameter and 30kg total samples
were collected from Educational Material Production and Distribution Enterprise center;
the collected samples were taken and the laboratory test processed. Experiments have been
conducted with varying influential process parameters to got different responses. Second
degree polynomial models for the responses as a function of the independent variables were
generated and optimum conditions were determined using Central Composite Face Cen-
tered Design of Response Surface Methodology.The data were analyzed to determine opti-
mum conditions for testing responses parameters particle size (90,70 and 45 m), calcina-
tions temperature (135, 140 and 145 o C) and moisture content (5, 6, 7%); for testing the
responses bulk density((1.121 - 1.201g/cm3 ) and breaking strength (10 - 20N/cm). The op-
timum value 1.1445g/cm3 bulk density of and 13.85N/cm breaking strength were achieved
at the optimum process parameters 85.55m particle size, 137 o C calcinations tempera-
ture and 6.25% moisture content. Depending on the optimum conditions determined ex-
perimentally and the existing condition of the plant, chalk production plant process flow
sheet has been proposed and the equipments have been designed in which case most of the
equipments can be easily fabricated locally. Finally, the plant is financially evaluated and
its initial investment cost will be recovered fully within only three years, which makes the
plant viable.

Key words: Gypsum, Plaster of Paris, Response Surface Methodology, Chalk

viii
1 INTRODUCTION

1.1 Background
Gypsum is sedimentary rock which settled through the evaporation of seawater trapped
in lagoons of subsoil and is usually found in mountains. It was formed when seawater
evaporated on the earths surface. Before that, sea levels were much higher than they
are today. As climate changed and sea levels lowered, seawater on what is now dry land
evaporated, leaving gypsum deposits behind. It is the only natural substance that can be
restored to its original rock-like state by the addition of water alone [1].

Ethiopia is rich with natural resources including gypsum but has no enough gypsum
plaster industry for construction purposes while it is abundantly used all over the world.
According to the available literature, gypsum plaster and its products are energy saving,
fire resistant, good insulating, cost effective and possess excellent thermal, acoustical
and aesthetic properties [2].

Chalk was first formed into sticks for the convenience of artists. The method was to
grind natural chalk to a fine powder, then add water, clay as a binder, and various dry
colors. The resultant putty was then rolled into cylinders and dried. Although impurities
produce natural chalk in many colors, when artists made their own chalk, they usually
added pigments to render these colors more vivid. For example, Carbon was used to en-
hance black, and ferric oxide (F e2 O3 ) created a more vivid red [2].

An important change in the nature of classroom chalk paralleled a change in chalk-

boards. Blackboards used to be black, because they were made from true slate. Man-
ufacturers began to fashion chalkboards from synthetic materials during the twentieth
century and they chose the color green, arguing that it was easier on the eyes. Yellow
became the preferred color for chalk[3].

The plaster of Paris and chalk manufacturing plant was established in 1970 year under
the education office of the Shoa Province and rehabilitated in 1982. Although significant
changes have been made to improve the production capacity and the quality of the out-
put, there remains much to be done in terms of quality and quantity in order to satisfy
the country plan [4].

1.2 Statement of the Problem

Ethiopia is one of the developing countries with a big rich resources, high population and
containing many of the under employed adults [4]. The country has been implement-
ing different strategies to bring these unemployed people to employ. Diversification of
jobs, increasing the availability of different product through domestic production, and

1
encouraging the production of high yielding products in different regions of the country
are some of such strategies.

It is obvious that the Ethiopian government has launched the growth and transforma-
tion plan. To meet this plans, the country requires educationally transformed genera-
tions. The education process at all levels needs educational supportive materials, one of
these supportive materials is writing board chalk.

Even if the technology of producing chalk is already there in the country, the existing
product do not favor the quality, performance and features. Therefore, characterization
of the scale helps to direct attention towards the component(s) responsible for the for-
mation of the optimizing and to assess the source of the raw materials. Even though, the
raw materials is locally available; our country is importing chalk from different countries
that incur foreign currency. In the recent year, the country started to use the locally avail-
able raw materials but still the quality is not as such good. It is known that educational
sectors in the country, be it private or governmental needs a good quality of writing chalk.

The major problems of chalks observed during use are:

too dry and difficult to write with

fragmentsizes easily and turns to dust or powder

difficult to wipe from the board

emits a shrill, piercing and scratching sound when applied on the blackboard

not uniform or consistent in quality

found broken pieces in the package

Due to these shortcomings, teachers and others who use the chalk are dissatisfied. This
is due to use of poor quality of raw materials and processing parameters, and equipment
design. This thesis is dedicated to produce improved quality chalk using locally available
raw materials; to investigate the effect of different process parameters such as tempera-
ture, types of raw materials, particle size, and moisture content and processing time. The
thesis will also to determine the optimum process parameters for high quality product.

1.3 Objective
1.3.1 General Objective

The general objective of this thesis work was to optimize the gypsum processing param-
eters for the production of improved quality chalk using locally available raw materials.

2
1.3.2 Specific Objectives

The specific objectives of the thesis were the following:

To study compositional analysis of raw materials.

To optimize the processing parameters.

To produce high quality of gypsum powder.

To minimize the dust of the product.

To test the quality of product.

To study the technical and economic feasibility.

1.4 Significance of the Study

Finding of the research adds to the knowledge and understanding of the production of
chalk using locally available raw materials in spite of importing. It can expand the tech-
nology in the country and help the people to get quality chalk in a simple way [3].
This study should be significant in the sense that:

Produce low cost chalk by using locally available raw materials.

Investigate the potential of gypsum under different process conditions.

Provide useful knowledge on factors that might have impact on quality of chalk.

3
2 LITERATURE REVIEW

2.1 The Structure of Gypsum System

Gypsum is a soft sulfate mineral composed of calcium sulfate dihydrate, with the chem-
ical formula CaSO4 .2H2 O and the most abundant sulphate mineral. It is water-soluble
and forms by evaporation or because of the mineral anhydrite being hydrated. These
unique evaporative and soluble properties are two factors, among many others that have
led to the unlikely formation of the largest gypsum sand dune field in the world [5]. The
presence of gypsum on or just below the surface of the ground is often indicated by
changes in vegetation; some plants thrive on gypsum-rich soil whereas others are not
at all tolerant of those conditions [6].

As shown in figure 1, the gypsum crystal, which has a monoclinic structure, is made up
of layers of calcium atoms and sulphate groups, separated by sheets of water molecules.
Ionic bonding forms the CaSO4 layer, while the water layer is formed by hydrogen bond-
ing. This structure provides the explanation for the ease with which crystals of selenite
can be split into layers (cleavage), because the plane of cleavage parallels the planes con-
taining the water molecules[7].

Figure 1: Schematic illustration of the layer structure of gypsum [7]

As shown in figure 2, each calcium ion is coordinated by six oxygen atoms of the sul-
phate group and by two water molecules. A three dimensional X-ray structural analysis
conducted by [8] has revealed that significant departure of the CaSO4 ion from tetra-
hedral symmetry occurs. The tetrahedral symmetry increases after removal of water
molecules, the S-O distance becomes uniform in natural anhydrous calcium sulphate
[9].

2.2 Geological Occurrence and Abundance of Gypsum

Gypsum is a mineral available all over the world but the main sources are the United
States, Canada, France, Italy and Britain. It forms as an evaporate mineral and as a hydra-
tion product of anhydrite. It occurs in extensive masses of great thickness, in association
with limestone and shale and in evaporative deposits; it is very soft and this is one of the
easiest methods of distinguishing it from other minerals such as limestone. Its deposits

4
Figure 2: Section of the crystal structure of gypsum; the horizontal dotted line shows the
plane of cleavage through the water molecules[9]

are found in water marine evaporates, caves where the air is dry enough for deposits to
form, areas where the earths crust has opened and occasionally in oxidized areas of sul-
fide deposits. It can also be prepared by precipitation from solutions of calcium salts and
sulphate at room temperature or by allowing plaster to set in water[10].

Gypsum is found in mineral and rock form. As a mineral, it can form very pretty and
sometimes extremely large and crystals. As a rock, it is a sedimentary rock typically found
in thick beds or layers. It forms in lagoons where oceans waters high in calcium and sul-
fate content can slowly evaporate and be regularly replenished with new sources of wa-
ter. The result is the accumulation of large beds of sedimentary gypsum. Because it is
deposited in this environment, it is common for gypsum to be associated with rock salt
and sulfur deposits [11].

2.3 Occurrence of Gypsum in Ethiopia

In Ethiopia, gypsum is formed by the hydration of anhydrite at or near surface, but usu-
ally passes into anhydrite below 40-50 meters, although this varies according to local
geological conditions. In nature gypsum occurs as beds or nodular masses up to a few
meters thick and is the products of the evaporation of seawater[12].

Gypsum has a history of usefulness to man dating back several thousand years. The lit-
erature review was referred to compare the three gypsum occurrences. These are Derba
Mugher site, Filiklik (Blue Nile Gorge) and Yogef (Jimma River) valley. Gypsum resources
are known to occur in Kentry, Filiklik, Blue Nile gorge, Yogef and Jimma River. These
gypsum occurrences are mainly associated with the Mesozoic sedimentary rocks and
encountered as intercalations with calcareous strata. To determine commercially ex-
ploitable gypsum resources that are suitable as a raw material for POP and chalk produc-
tion, the aforementioned three gypsum occurrences were assessed and evaluated here-
under regards to location and access, mode of occurrence, quality and resource (reserve)
assessments[13].

[a] Kentry Gypsum Occurrences: There are two gypsum beds, having thickness of 4m
and 12m, respectively with a 4m intercalation of sandstone in between. Kentry is

5
 geographically located North West of Addis Ababa. The chemical analyses of this
gypsum are (25.56 - 38.54%)CaO, (25.06 - 54%) SO3 and (9.09 - 18.08%) H2 O [14].

[b] Filiklik (Blue Nile Gorge) Gypsum Occurrence: Filiklik gypsum potential target area
is geographically situated North West of Addis Ababa. This can be reached by 202
km asphalt road, along the way through Addis Ababa-Debremarkos highway. The
potential of target area of gypsum that is investigated at prospection level is situated
about 500 m west of the mining area of gypsum to the left of the main road to Abay
Bridge. The gypsum occurrences are morphologically hill forming. The chemical
analysis of this gypsum are: (38.30-36.24%) CaO, (51.38-48.78%) SO3 and (10.35-
11.94%) H2 O [14].

[c] Yogef Gypsum Occurrence: The Yegof gypsum deposit occurs in Jema valley near the
confluence of Jema and Bedrsina rivers situated North of Addis Ababa. The gypsum
is cliff forming with sharp edges, sacrificially showing rill marks.

Table 1: Compositions Yogef gypsum occurrence[15]

Description CaO(%) SO3 (%) H2 O (%) LOI(%) SiO2 (%) Fe2 O3 (%) AlO3 (%)
Lower gypsum 28.55- 43.23- 14.63- 5.00- 0.70- 0.09- 0.08-
bed 31.75 45.94 17.34 5.97 1.00 0.15 0.14
Upper gypsum bed 0.12- 4.68- 17.97- 3.5- 0.65- 0.07- 0.09-
bed 31.22 45.76 18.89 4.21 0.82 0.10 0.12

According to different literature reviews, gypsum rock has the following composi-
tions of 32.6% CaO (Lime), 46.5% SO3 (Sulphate) and 20.9% H2 O (water) when very pure.
Therefore, the average chemical compositions of gypsum samples collected from the
aforementioned occurrences should be evaluated and compared with these ranges of
values[16].

According to the information from Ministry of Mining the present annual consump-
tion of gypsum rock (raw material), the existing plant uses the amount of 1,000 - 1,500
tons for POP and chalk production purposes. Therefore, the occurrences of the gypsum
rock in the above-mentioned localities shall be future potential resources for plaster of
Paris and chalk production, including other small and medium scale gypsum processing
plants[17].

2.4 Production of POP and Chalk in Ethiopia

2.4.1 Production of Plaster of Paris

In Ethiopia POP had been producing and marketing since 1986 year and the productions
of data spanning the period 2007-2013 are shown in the Table 2. As it can be seen from
the table, the production of POP was increasing from year to year.

6
 Table 2: Production of POP in Ethiopia in consecutive ten years
Year (G.C) 2007 2008 2009 2010 2011 2012 2013
Quantity Production(Ton) 438.5 650.2 559.8 944.2 1058.23 1263.45 1511.87

Sources: EMPDE

Since the bulk of demand for POP is not met through local production with the qual-
ity and quantity wanted, it imported from different countries for various purposes. The
POP imported from overseas is generally of higher quality and fineness and it is mainly
used for medical (bone casting), ornamental and industrial uses. An enterprise AJECA is
known to import gypsum from Jordan for sales to the construction market.

Table 3 shows that the imported of Plaster of Paris during the period under considera-
tion is characterized by high fluctuations. The imported data ranges from 4.5 tons and
6.5 tons in the year 2012 and year 2013 respectively to 108.6 tons in 2009. In the remain-
ing years, it ranged from the lowest 15.7 tons in 2011 to the highest 58.5 tons in 2008. The
average imported of POP of the last four years was about 75 tons, which is not that much
significant compared to the locally produced Plaster of Paris in the recent years.

Table 3: Imports of Plaster of Paris

Year (G.C) 2007 2008 2009 2010 2011 2012 2013
Quantity Imported (Ton) 23.3 58.5 108.6 37.4 15.7 6.4 4.5

Source: Ethiopian Revenues and Customs Authority

2.4.2 Production of Chalk

Chalk is used in school and other learning establishments to write on the board. The
demand for chalk is high and this has made its production a goldmine. Common black-
board chalk, which was traditionally made from natural chalk, today is made from gyp-
sum. Blackboard chalk is made into sticks and used to draw on blackboards and other
rough surfaces. EMPDE had remained to be the sole domestic producer of chalk in
Ethiopia for many years. Other producers of chalk came into market only about five years
ago, but their number and capacity is growing from time to time [18].

Table 4: Production of Chalk in Ethiopia in consecutive five years

Year (G.C) Production (Gross) Production (kg)
2009 263,368 184,358
2010 313,000 219,100
2011 361,364 252,955
2012 368,296 257,807
2013 388,416 271,891

Source: FDRE Ministry of education

7
 To convert from kilograms to gross, one gross is equal to 700 gram and one piece of
chalk is 6.7 gram. As the data showed in Table 4 and Figure 3, the capacity of the product
was increasing from time to time.

Figure 3: Production Chalk in Ethiopia

The minimum and maximum productions of chalk in the past five years were 263,368
gross in 2009 and 388,416 gross in 2013 respectively. The average production during five
years was 32,5892 gross and the corresponding average annual growth of production was
3.2%. This is because of the expansion of school in the country very rapidly. On the other
hand, chalk was imported into the country from France, India, UK, Germany, Taiwan,
Thailand and Netherlands for many years.

Table 5: Quantity of Chalk Imported

Year (G.C) Quantity Imported (Gross) Quantity Imported (kg)
2009 366,925 35,401
2010 404,488 39,025
2011 231,478 22,333
2012 225,676 22,756
2013 198,979 20,064

Source: Customs and Excise Tax Authority, External Trade Statistic, Annual Issues

2.5 The Physico-Chemical properties of Gypsum

Characteristics of gypsum include a low hardness level, perfect cleavage and a mono-
clinic crystal system of vectors with unequal lengths. Gypsum is a mineral with thick
and fine tabular type crystals, large crystals being very rare, crystals are flexible but not
elastic, which means that you can bend but they do not spring back, they stay bent. The
aggregates are compacting granular, foliated and fibrous. It is a soft mineral and a fin-
gernail can scratch its crystals, which is about the only test needed to distinguish it from
other minerals that have a similar appearance. The color of gypsum when reduced to
powder is white. The specific gravity of gypsum, i. e., its weight as compared with pure
water, is 2.3[19].
Identification: gypsum is the most common sulfate mineral. It is common to find gyp-
sum with calcite, sulfur, halite and anhydrite in layers of sedimentary deposits[20].
Color: Pure gypsum is a white-to-transparent mineral, though impurities can give the

8
mineral a yellow, grey, red, brown, pink or colorless[21].
Shape: gypsum forms as granular masses, fibrous masses, tabular shapes and prisms.
Twin also knows gypsum, to form mirror image crystals on the same level. It is classified
under the monoclinic crystal system [22].
Hardness and breakage: minerals are rated using the Mohs scale of hardness. The hard-
ness of gypsum varies from 1.5 to 2.0, the crystalline form being taken as the standard for
the second degree in the scale of hardness of minerals[23].
Conductivity: It is a poor conductor of heat, which makes it useful in wall board and dry-
wall which makes it a good insulator[24].
Chemical Formula: Its chemical name is calcium sulfate dehydrate, and its chemical for-
mula is CaSO4 .2H2 O which means that every dry gypsum molecule has trapped within
itself, two loosely attached molecules of water that can be driven off simply by heating it
up beyond the boiling point of water[19].

Table 6: Physical and chemical properties of gypsum

Characteristics Properties Descriptions
Class Sulfates 35,401
Chemistry CaSO4 .2H2 O It has oxygen, calcium,
sulfur, and hydrogen in it.
Crystal System - Monoclinic - prismatic
Crystal Habits - Include the tabular, bladed or
blocky crystals with a slanted
parallelogram outline.
Fracture Conchoidal and splintery This mineral does not break ,
into pieces often but when it does
it does not do it evenly.
The splinters would be smooth.
Hardness 2 Mohs scale It is so soft
that a fingernail can scratch it.
Specific Gravity 2.3 It is a very light stone.
Luster Vitreous to pearly When light shines on it,
it looks glassy or pearly.
Streak White When the stone is rubbed on a white plate,
it leaves a white powder.
Cleavage Good in one direction If you hit it with a hammer,
it would break into layers
going in one direction.
Field Indicators - Are crystal habit,
flexible crystals, cleavage and hardness.
Associated Minerals - borax, calcite,
halite, pyrite, sulfur and others

(Source: Wikipedia encyclopedia)

Mineral gypsum exists in variety different forms[25]:

Selenite - Selenite is composed of well-developed crystals, is colorless and trans-

parent, and has a pearl like luster.

9
 Alabaster - Pure alabaster is a fine-grained massive material which is white and
compact. It is commonly carved and polished for statues and ornaments.

Satin Spar - Satin Spar is a fine translucent variety composed of monoclinic crystals.
It is valued for ornaments and jewellery.

2.6 Technology Selection and Production Process of POP

2.6.1 Size Reduction Process

Gypsum rock from the store is transported by a loader and fed to the hopper, then con-
veyed by a feeder and belt conveyor to the jaw crusher. This is passing through two pro-
cesses: jaw crusher and small crusher. Primary crushing crush gypsum stone into smaller
particles; the general control of particle size is less than 10cm. The larger particles will
have re-crushed and smaller particles will be convey by the belt conveyor into the sec-
ondary crushing with a hammer crusher machine to control the particle diameter less
than 28mm and then transfer by the bucket elevator into the grinding mill[26].

Secondary crushers that work at higher speeds, producing pebbles, accomplish secondary
crushing. The crushed gypsum is stored in the hopper from where it is conveyed using
a belt conveyor and fed to the hammer mill for further grinding; the ground gypsum is
discharged to the hopper and further transported by screw conveyor and bucket elevator
to the storage silo. The finely ground gypsum ore is known as land plaster[27].

2.6.2 Kettle Calcinating

There are two distinct types of kettle calcinating technologies, namely; continuous and
batch kettle calcinating. However, the only feasible calcinations for small-scale plant is
batch kettle calcinations. The land plaster is transported by screw conveyor and bucket
elevator and fed to the kettle calciner where it is heated to remove three-quarters of the
chemically bound water to form POP. Calcinations occurs approximately 130 to 150o C
and the time taken for calcinations is about two and half hours. During the process of
calcinations, the gypsum loses 75% of its moisture thereby making it hydroscopic[28].

There are different types of calcinations necessary to produce POP, but in this paper
only the kettle calcinations is used. Because kettle is simple to design and used to hold
up to 15 kuntals per batch. Roller mills prepare raw gypsum rock for introduction into
calcinating kettles by simultaneously removing the surface moisture. The kettles effi-
ciently remove chemically bound water from the raw gypsum by heating and agitating it
in a carefully controlled process. The resulting product, homogenous calcinated stucco
is eminently suitable for use either in manufacturing wallboard or in plaster applications
[30].

10
 Figure 4: The process flow diagram of POP production line[29]

In the kettle calciner, the plaster is indirectly heated by hot combustion gas passed through
flues in the kettle and the product is discharged to hopper located below the kettle. The
plaster is conveyed by screw conveyor and put into the hopper for feeding into the pul-
verizer. The plaster is further ground in pulverizer and transferred to storage silo by screw
conveyor and bucket elevator. Packing of POP using plastic bags is carried out at the bot-
tom of the storage silo [31].

2.6.3 Plaster of Paris (POP)

The calcium sulphate dihydrate becomes commercially useful substance by calcinating

(i.e. driving out the chemically bonded water) using heat and then grinding it to the re-
quired grain size (or fineness)[30]. Chemically, Plaster of Paris is calcium sulphate having
molecular formula CaSO4 .1/2H2 O. It is a white hygroscopic powder very slightly solu-
ble in water particularly at high temperature. The principal of POP manufacturing is to
convert gypsum, dehydrate form of Calcium Sulphate to POP, hemi-hydrate of Calcium
sulfate by controlled heating. Hence, production of POP involves dihydration of gypsum
and preparing it in usable form (powder)[31].

Based on end use application and heats of hydration two types of POP are produced
namely, Alpha and Beta-type POP. Alpha-type is characterized by crystalline nature while
Beta-type of is characterized by amorphous nature. After vigorous mixing of the hemi-
hydrates with water, a typical beta hemihydrates plaster require between 75 to 100ml of
water per 100g of plaster to give pourable slurry. A typical alpha hemihydrates, on the
other hand require only 28 to 45ml of water to give pourable slurry with 100g of plas-

11
ter[32].

Calcinations under atmospheric pressure to produce Beta plaster, and

Calcinations under elevated pressure to produce Alpha plaster. Each category of

calcinations of gypsum into plaster was described briefly as follows.

Beta Plaster: Beta plaster presents micro-crystals that yield high porosity and average
low mechanical strength only when cast with water, as they need high excess of water
in slurry (typically water quantity will be 80% of plaster quantity). The type of plaster
required for manufacturing chalk is the beta plaster[33].
Alpha Plaster: Alpha plaster presents well formed crystals that will yield low porosity
and high mechanical strength when cast with water, as they need high excess of water in
slurry (typically water quantity will be 33% of plaster quantity)[34].

Table 7: Comparison of alpha and beta plaster

Properties Alpha process Beta Process
Mechanical strength Higher Lower
Crystals Larger Smaller
Porosity Lower Higher
Specific surface Lower Higher
Water demands Lower Higher
Density Higher Lower
Energy Higher Lower
Heat reaction Larger Smaller
Calcinations Temperature Up to 150o C Up to 300o C
Pressures Higher than atmospheric pressures At atmospheric pressure

The hemihydrates are probably so named because of the very large deposit of pure
gypsum found beneath Paris. It can be mixed with water, spread and cast into different
forms and sizes. Being a hygroscopic material (i.e. containing water), calcium sulphate
dihydrate undergoes chemical decomposition reactions when heated and the water of
crystallization is driven off some or all of the water of crystallization. POP is a chemical
having the notable property of setting and subsequent hardening when mixed with wa-
ter[35].
The chemical endothermic reaction is:

CaSO4 .2H2 O + Heat CaSO4 . 21 H2 O + 1.5H2 O

During this reaction, gypsum dihydrate to calcium sulphate hemihydrates (or POP) and
75% of the chemically combined water is released. With further increase in the tempera-
ture, the remainder 25% of the chemically bound water.

CaSO4 .2H2 O + Heat 7 CaSO4 + 2H2 O

Rehydration
If the powder is mixed with water to form a slurry or paste, it dry and set rock hard. As the
plaster and water, mixture dries, water is chemically recombine with the hemihydrates

12
gypsum and the material revert to the original composition of gypsum. The basic rehy-
dration reaction is the reverse of calcinations. POP consists of a fine, white powder and
calcium sulfate hemihydrates that hardens when moistened and allowed to dry [36]. To
convert the reaction above by mixing gypsum product (powder) with water:

CaSO4 .1/2H2 O + 3/2 H2 O 7 CaSO4.2H2 O + Heat

When the POP is mixed with water to a pourable state and allowed to set; it reverts back
to a solid mass. This process is called recrystallization. The material heats and expands
until it reaches the chemical composition of natural gypsum-containing two molecules
of water. Certain modifiers can be added to the plaster to accelerate or retard the setting
process [37]. Generally, the following reaction can take place in gypsum powder produc-
tion:

CaSO4 .2H2 O(s) 7 CaSO4 .1/2H2 O(s) + 3/2 H2 O (L)

CaSO4 .2H2 O(s) 7 CaSO4 (s) + 2H2 O (L)
CaSO4 .1/2H2 O(s) 7 CaSO4 (s) + 1/2 H2 O (L)
CaSO4 (s) + 1/2H2 O (L) 7 CaSO4 .1/2H2 O(s) (slow)
CaSO4 .1/2H2 O(s) + 3/2H2 O(L) 7 CaSO4 .2H2 O(s) (fast)

2.7 Gypsum Dehydration Sequence

Plaster is produced from the dihydration of gypsum. Calcium sulphate dihydrate (here-
after referred to as dihydrate) dihydrate on heating to calcium sulphate hemihydrates
(hereafter referred to as hemihydrates). The -hemihydrates is produced by dry calci-
nations and is the main constituent of plaster. The -hemihydrates is produced by wet
calcinations at elevated pressures or atmospheric pressure with the addition of acid or
aqueous salt solutions. Hemihydrates on heating dehydrate further to calcium sulphate
anhydrite (hereafter referred to as anhydrite) [38].

The important physical properties of the different calcium sulphate phases were shown
in Table 9. Calcium sulphate hemihydrates occur in and forms. Plaster consists on
the whole of the -hemihydrates form, which is made up of flaky rugged secondary par-
ticles. The -hemihydrates consists of compact, well formed, transparent, large primary
particles. The properties of hemihydrates can lie anywhere between those of the two end
members depending upon the water partial pressure when formed[39].

Table 8: Phases of gypsums

Calcium Sulphate Chemical Formula Abbreviations
Dihydrate CaSO4 .2H2 O D
Hemihydrates CaSO4 .1/2H2 O H
Anhydrite III CaSO4 AIII
Anhydrite II CaSO4 AII
Anhydrite I CaSO4 AI

13
 At high temperatures, dihydrate can be dihydrated directly to anhydrite. Anhydrite
exists in 3 forms, AIII, AII and AI depending upon the temperature of reaction. AIII
is meta-stable at ambient conditions and will readily rehydrate to hemihydrates in the
presence of water vapor. AII is stable at ambient conditions and AI is not stable below
700o C[40].

Factors affecting the rate of dehydration

It has been found that the rate of the dehydration reaction increases with[41]:

Increasing temperature

Decreasing particle size

Decreasing water vapor pressure

Decreasing air pressure

Figure 5: Plaster production process

For the plaster stage, various types of gypsum are produced by differentiating the tem-
perature of the calcining process. Higher temperatures lead in general to a lower reaction
with water[42]. As the temperature is increased, the reaction rate increases and there is a
greater possibility of the formation of the undesirable anhydrite phases. Gypsum, hemi
and anhydrite can co-exist within a single grain of gypsum, with the thickness of each
successive layer depending upon temperature, rate of heating, particle size, moisture
content and possibility of rehydration.

14
 Table 9: Physical properties of gypsum, hemihydrate and anhydrite
Properties Dihydrate Hemihydrates AIII AII AI
Formula CaSO4 .2H2 O CaSO4 .1/2H2 O CaSO4 CaSO4 CaSO4
MW(kg/kmol) 172 145 136 136 136
Crystallization 21Wt% 5.25Wt% 0 0 0
Density, kg/m3 2,310 : 2,757, 2,580 2,930 - 2,970 Not known
: 2,619-2,637
Solubility 0.21 :0.67, : 0.88 D to H 0.27 -
Hardness, Mohs 1.5 - - 3-4 Not known
Thermodynamic <40o C Metastable Metastable 40-700o C >700o C
Forms/Stages - 2 forms, , - - -
Synthesis :<40o C : >40o C, - 200-700o C >700o C
Conditions :45-200o C
Production Temp <40o C : 80-150o C, - 300-600o C Not
:220-300o C produced

The dihydration of dihydrate and hemihydrates is strongly influenced by water vapor

pressure. If the water vapor pressure is high, enough at a given temperature then the
dehydration reaction does not proceed[43].

Table 10: Hemihydrates, anhydrates, and respective calcining temperatures[36]

Name Chemical Formula Calcining Temperature
-hemihydrate CaSO4 .1/2H2 O 130-150o C (saturated steam atmosphere)
- hemihydrate CaSO4 .1/2H2 O 220-300o C (standard atmosphere)
-Anhydrite III CaSO4 .0,xH2 O 290o C(saturated steam atmosphere)
-Anhydrite III CaSO4 .0,xH2 O 110o C (standard atmosphere)
Anhydrite IIs CaSO4 300 - 500o C
Anhydrite IIu CaSO4 300 - 500o C
Anhydrite I CaSO4 >700o C

2.8 Technology Selection and Production Process of Chalk

At present, the basic difference between different technologies of producing school chalk
is in its being automated or manual production. In the manual production, chalk is pro-
duced by moulding on 600 pieces moulding machines. Drawing of the chalk is done by
pushing the piston using a mechanism assembled on the moulding machine at the bot-
tom of the cylinders manual pushing handle. Drying the chalk is carried out by hot air
heated by kerosene/diesel oil[44]. The advantage of manual chalk production plant is
that there is not be plant stoppage if one of the machines stops operation, except the
dryer. Its disadvantage is that the efficiency and quality is depending on the dedication
of the operators.

In the automatic production, chalk is produced by moulding on cylindrical rubber moulds.

The moulding is carried out on closed ring chain conveyor and lasts about 12 - 15 min-
utes. At the end of the round path, the hardened school chalks are taken out by means
of automatic draw machine and automatically put on moving trays. The chalks on trays

15
get into constant and continuous cycle dryer. Drying is carried out by burning the LPG.
The dried chalk is automatically filed into carton boxes and packed. The whole plant
is controlled by an operative control system[45]. In automated plant, there is no prob-
lem on the quality of the product and on its efficiency since each operation is controlled.
However, the plant is forced to stop if one of the machines is out of operation by any rea-
son. Besides, running costs of fully automated plant of a continuous type production in
Table 11: Specification of chalk
Physical and chemical properties Description
Appearance White crystalline powder
Specific Gravity 1.14
CaO 39.1%
SO3 53.2%
F e2 O3 0.25%
H2 O 5.5%
Heat capacity, Cp 0.9kJ/kg.K
Density of chalk 1.14g/cm3
Calcinations temperatures 135o C
Calcinations time (110 - 130) minutes
Molding time (12 - 15) minutes
Particle size 90m
Drying time 480 minutes
Drying temperature 120o C
Moisture contents 7%
Mass of 1 piece of chalk 6.7gm
Diameter of 1 piece of chalk 10mm
Length of 1 piece of chalk 80mm
Bulk Density (1.121 - 1.201)g/cm3
Breaking Strength (10 - 20)N/cm

terms of maintenance cost and complexity, cost of fuel, etc are higher than that of man-
ual plant. However, product quality, operation efficiency, unitary machines output, etc.
are higher for an automated plant [46].
1. Manual Batch- type production of chalk
Correctly, measured amount of water using a handle is poured into the stirring tank.
Then the raw material, calciner is correctly measured on a scale and is poured into the
stirring tank. Mixed oil is painted with a brush on the inner side of the mould before-
hand. The milky slurry mixture is passed through 90tm filter and filled into the mould.

The work from stirring the raw material up to finishing the moulding is done in 60 - 80
seconds. In order to minimize the bubble in the mixture which has been poured into the
mould, the moulder is given a slight jar to release the air bubbles from the top. The ra-
tio of mixed oil used as mould releasing agent is 200 liters of kerosene to 3 liters of any oil.

The time to draw out the chalk is approximately 12 - 15 minutes after moulding. When
the chalk is ready to be drawn out of the moulding machines, a drawing frame is placed
on the top of the moulding frame and the moulding machines is inclined 90 degree, then

16
the chalk is automatically fall into the drawing frame.

The drawn chalk is taken away, and put in a designated place, arranged in a drying

Figure 6: The process flow diagram of batch- type manual chalk production line[47]

frame and then dried in the drier. The dried chalk is then packed in a carton manually.
The advantages of using manual batch-type plant are that it is simple to operate with
relatively low running costs like cost of maintenance, spare parts and source of power.
The main disadvantages are lower unit output of production equipment, especially the
moulding machines, stirrers, etc. and inferior product quality[48].

2. Automated Continuous- type production of chalk

The plaster from silo, silo is discharged by screw conveyor and fed into an automatic
mixer. Water is simultaneously poured into the automatic mixer with an electronic pump
which regulates the water flow rate. The raw materials are measured accurately and
mixed in the mixer. The automatic mixer pours the already automatically pre-mixed
plaster mixture into special rubber moulds. The moulds have the pre-selected shape
according to the type of school chalks and lie on a transportation line composed of mo-
bile cars[49].

After pouring the plaster mixture into the shapes, a closed-ring, linear, horizontal pro-
cess was started lasting about 14-17 minutes. At the end of the round path, the already
hardened school chalk is removed by means of an automatic pattern draw machines and
automatically put on other flat moving trays. The chalk on the trays then gets into the
constant and continuous cycle dryer. At the dryer output, a selection of the product takes

17
place by means of an automatic optical system where the damaged product is scrapped
while the equality one is automatically placed into 144 unit boxes. Then the boxes are
stored in a warehouse.

The automatic continuous-type plant has the advantage of high unit output of equip-
ment and quality final product. High cost of spare parts, maintenance and power are
among the disadvantage of the automatic continuous-type production of chalk. How-
ever, the advantages of the automated continuous-type production technology overweigh
its disadvantages[50].

Figure 7: The process flow diagram of automated continuous-type production line

2.9 Different Processing Parameters on Chalk

Functional properties refer to physical and chemical properties of a chalk or chalk com-
ponent that affect the quality of the product. Parameter processes of chalk produc-
tion such as particle size, temperature, time and moisture content predict the functional
properties of products[50].
The most important dependent variables after processing are the product quality char-
acteristics. Yield strength and bulk density are related to these parameters in different
ways. As the size of the particle decreases, the time taken to evaporate the moisture con-
tent from the raw materials decrease. This means the moisture content of the gypsum
powder evaporate by a minimum temperature. The high dependence of bulk density
and yield strength on temperature would reflect its influence on the quality of the prod-
uct. As temperature increases, the moisture content during calcinations decreases and

18
the time increases. Therefore, decrease in particle size decreased yield strength and in-
creased bulk density[51].

The properties of gypsum during size reduction process are influenced by the machine
variables (e.g. types of the machine and design), the parameter processing variables (e.g.
calcinations temperature, calcinations time, moisture contents and particle size) and
types of raw materials used. The interaction among all these variables transforms the
feed materials leading to the changes in product qualities[52].

2.10 Other Possible Raw Materials to Produce Chalk

There are other possible raw materials in the country to produce chalk. These raw ma-
terials are dolomite and calcium carbonate. Dolomite is a common rock-forming min-
eral. It is a calcium magnesium carbonate with a chemical composition of CaMg (CO3 )2 .
Chemically dolomite is a double carbonate of calcium and magnesium with a pronounced
crystalline structure. However, the problems with these raw materials are that they need
maximum temperature for calcinations and have many problems on the environmen-
tal[53].

2.11 Application of Gypsum

The most general use of gypsum products is in those structures where their lightweight
and fire-resistant qualities make them especially desirable. It is used to retard the setting
time of cement (average 3 - 6% added to the clinker), as a fertilizer, as a source of calcium
and sulphur and as soil conditioner. It is also used as a substitute for sodium sulphate
in glass making. It is inert with good absorbing capabilities. Together with inertness and
lack of abrasiveness, some grades of gypsum are sufficiently pure to be used as a filler or
diluents in paint, plastics, textiles, food and pharmaceutical industries[54].

Best quality, finely ground white gypsum is used as a base in cold-water paints and in
the manufacture of certain cheaper grades of pigments. Plaster of Paris is a basic ingre-
dient of many plastic paints as a hardening agent being added to make the material more
durable. In the textile industry, gypsum in its ground form is used in the finishing of cot-
ton and cloth to give weight to a product when a lustrous or glossy surface is required[55].

Calcined gypsum is also widely used in the pottery industry as moulding plaster. In den-
tistry and orthopedics, gypsum is used as a moulding and casting material. Plaster board
or gypsum board, which consists of sheets of slabs of gypsum mixed with fibers, is em-
ployed as fire resistant material for walls, ceilings or partitions. In the chemical indus-
tries, gypsum is used in the manufacture of sulphuric acid and ammonium sulphate[56].

19
2.12 Environmental Implications
Gypsum crystal is usually found in conjunction with or near sulfur deposits. If the cal-
cium sulfates in gypsum mixes with the sulfur, then toxic chemicals can be produced,
so the gypsum must be mined properly to ensure the substances remain separate. One
chief use for gypsum is in drywall used to build houses. Contaminated gypsum inside
the walls of a house would jeopardize the health of the environment and surrounding
communities[55].

The process of extracting the gypsum from the ground can cause environmental degra-
dation. According to the Global Press Institute, gypsum mines in India leave scars on the
landscape. Not only are they unpleasant to look at, but all structure has been removed
from the landscape and deposits of gypsum are left exposed to the elements. The lack
of rock or vegetation leads to soil erosion and causes sinkholes and landslides. Exposed
gypsum dissolves easily in the rain and leaves gaping holes that both contribute to the
erosion and pose a physical danger [56].

The product does not create any noise or water pollution. The air pollution has to be con-
tinuously monitored. Masks can be used by the workers while making powder (grinding).
The production of plaster and plasterboard puts very little pressure on the environment.
The final product is non-toxic and wastage and unwanted by-products from the process
are minimal. The technology uses gypsum and fuel only and its waste product is mainly
gaseous water and carbon dioxide. So, the process is environmentally friendly [57].

20
3 MATERIALS AND METHODS

3.1 Time and Place of the Study

The study was conducted from October 2013 to October 2014 at Addis Ababa University,
Addis Ababa Institute of Technology: school of Chemical and Bio Engineering in Pro-
cess Engineering laboratory (AAiT) and the results were tested in Geological Surveys of
Ethiopia and Food Engineering Laboratory (Hawassa University).

3.2 Materials
The materials used to run the experiments are listed below:

Jaw crusher, Secondary crusher, Miller and Pulverizer - for size reduction of rock

Kettle - to evaporate the water contents from gypsum

Moulds -to shape the mixture

Scraper - for scraping the surface of the chalk mould.

Paint Brush - for applying lubricant on the mould before filling it up with POP.

Lubricants: It could be any cooking oil or coconut mixed with kerosene. Its purpose
is for lubricating the chalk mould to prevent the POP from sticking to it.

Ultramarine Blue and Fe2O3: This is used to give the chalk color but it is optional if
one is interested in producing only white chalk.

Sieves(mesh size of 45m, 70m and 95m Sortmks-3332, PFEUFFR, Germany)

with shaker -for size classification

A Spatula (Mingling stick)

A weighing Scale (grammometer)

Fuel - for calcinations

Tray Dryer - for holding the wet chalk sticks until they dry

3.3 Methods
3.3.1 Source and Preparation of Raw Materials Sample

Gypsum selection and preparation (cleaning and classifying) are the key factors to pro-
duce the best plasters and quality chalk. Gypsum rocks with size less than 20cm in diam-
eter and 30kg total samples were collected from EMPDE center, which is located in Addis

21
Ababa; the collected samples were taken and processed the laboratory test. All other ma-
terials such as paints, oils, gasoline, fuels, packaging materials etc. were bought from
local market. All samples were transported to Process Engineering laboratory of AAiT for
further works within 20 days.

3.3.2 Size Reduction of the Sample

The size of the taken samples was adjusted to less than 10cm in diameter by hammer.
In jaw crusher the sample was reduced to a size less than 5cm in diameter and further
reduced to a size less than 20mm in hammer mill. The particle size of the sample was
further reduced in grinding mill to less than 2mm which increased the amount of fine
particles in the powders. It is important to select proper grinding mill with high efficiency
and capacity [31]. Finally, the sample was pulverized to a particle size less than 120m
and the optimum size was determined. The sample was sieved using vibrating shaker
(Retsch) with set of sieves arranged in descending order 95m, 70m and 45m and this
is to investigate the effect of particles size on the quality of chalk [35] .

3.3.3 Calcinations Procedure

The grounded gypsums were calcinated in an oven within a temperature range of (135
- 145o C) and the calcinations temperature was chosen accordingly for all the samples.
The calcinations time was dependent on the working time of machine. When the kettle
starts work, it takes more time to evaporate the water content. As the machine stayed on
work for two and more batches, the time it takes was decreased. This is because when
the machine was very hot, the wanted temperature was arrived in a short time. For each
experiment, 500g of the grounded and sieved samples was weighed and put in an oven.
These samples was calcinated at different temperatures in the stated range until 70%,
75% and 80% of the moisture content was derived off in the form of vapor. Calcinations
temperature was measured by a thermocouple inserted along the length of the kettle
calciner [30].

3.3.4 Mixing Procedure

500gm of POP was weighed and mixed with 600ml of cold clean water in bucket and
white chalk was produced. 490gm of POP was weighed and mixed with 600ml of clean
water and 10gm of any wanted colors and colored chalk was produced which is standard
Worldwide [31]. It was mixed properly back and forth motion while turning the container
every once in awhile and made sure that the mixture is not watery and at the same time
not too thick. This will allow the POP to be evenly incorporated with the water. The sides
of the bowl must also be scraped to make sure there are no dry samples sticking to the
sides. The mixing was continued until an even consistency achieved. There should be no
lumps in the POP mixture. After mixing the POP with water, the resulting slurry must be

22
used within two to three minutes. POP when mixed with water tends to dry up fast. It is
best to have the moulds ready so that the slurry can be poured into them immediately; it
cannot be kept; it must be poured into mould otherwise it is wasted [44].

3.3.5 Moulding Preparation

The pieces of the mould should be washed very well with the mixture of oil and kerosene;
couple the mould together with the provided treaded rod and make sure they are tightly
closed to avoid leakage. The ratio of kerosene to oil mix used as mould realizing agent
kerosene to oil is 3:1 litters and painted with a brush on the inner side of the mould
beforehand. Pour the solution into the mould; shake the mould and use your hand to
guide the solution as you are pouring to ensure that it gets to bottom of the mould and fill
it properly. The solution should be poured at the center of the mould then using scraper
smear the mixture into mould hole. The slurry mixture remaining on the top surface of
the mould frame is wiped off with a metal spatula, and then the top surface of the mould
is rapidly finished off with a finishing spatula[45]. It is allowed the solution to stay in the
mould for 12 to 15minutes to give the shape of chalk and this is the first stage at which
the drying take place. When the chalk is ready to be drawn out of the mould, a drawing
frame is placed on the top of mould frame and the drawing stopper is set firmly. The
mould is inclined 90 degrees toward the operator and the chalks automatically fall in to
the drawing frame. The drawn chalks are then taken away, put in to the designed place,
and arranged in trays for drying[44]

3.3.6 Drying Procedure

Now the arranged trays were entered into the dryer and dried at 120oC. Moisture is re-
moved from water-based coatings and adhesives, as well as from the surface and interior
of products or substrates. Testing: Laboratory testing was carried out at several produc-
tion phases to ensure all products meet the strict product specifications before being
bagged and shipped.

3.4 Proximate Determination

All raw materials samples were analyzed in duplicate for their proximate composition
according to the following procedures.

3.4.1 Determination of Moisture Content

Moisture content was determined by drying the samples in an oven until a constant
weight obtained. The 500 grams of samples and 6grams of the aluminum foil; total of
506 grams were accurately weighed and put in kettle and dried at the 135, 140 and 145o C

23
temperatures. The process was repeated until a constant weight obtained [48]. The mois-
ture content was determined using equation. (1).

Weightofsamplebeforecalcination Weightofsampleaftercalcination
MC(%) = (1)
Weightofsamplebeforecalcination

3.4.2 Determination of Bulk Density

To determine the bulk density of the chalk, the chalk was weighed and put in cylinder
with clean water and stayed for 3 to 4 minutes. The wet chalk was taken from the water
and measured carefully [59]. Repeating this experiment three times and recording the
weight, bulk density of the chalk had been calculated as follows in equation (2):

MassofWetChalk(g)
BulkDensity(N/cm3 ) = (2)
VolumeofChalk(cm3 )

3.4.3 Determination of Breaking Strength

The chalks were placed on the sample platform of 1kg load cell with 2 - 6cm specimen
TA-XT plus texture analyzer. The load was released vertically to the chalk. The max-
imum force in Newton (N) required to break the samples exceeding a breaking limit
was recorded and the average of three samples was used for calculation. Hardness and
breaking strength of chalk was determined as the maximum force offered by chalk dur-
ing breaking and three point diameters [59]. The breaking strength was calculated using
equation (3):

BreakingForce(N)
BreakingStrength(N/cm) = (3)
Distanceb/nloadandchalk(cm)

3.5 Experimental Design of Process Parameters

Experimental designs nowadays have been regarded as one of the most favorable tech-
niques in covering a large area of practical statistics and obtain unambiguous results with
the least expense. An experiment is a series of tests, called runs, in which changes are
prepared in the input variables in order to recognize the reasons for changes in the out-
put response [60]. Design of experiments is a powerful technique used for exploring new
processes; gaining increased knowledge of the existing processes and optimizing these
processes for achieving world class performance and enable designers to determine si-
multaneously the individual and interactive effects of many factors that could affect the
output results in any design [61].

Optimizing refers to improving the performance of a system, a process, or a product in

order to obtain the maximum benefit from it. Often engineering experimenters wish
to find the conditions under which a certain process attains the optimal results. i.e., by
careful design of experiments, they want to determine the levels of the design parameters

24
at which the response reaches its optimum. The optimum could be either a maximum;
a minimum or target responses which is influenced by several independent variables
(input variables). One of methodologies for obtaining the optimum results is response
surface methodology [62].

Response surface method (RSM), invented by Box and Wilson, is defined as a collection
of mathematical and statistical tools or techniques useful for modeling, analyzing and
simultaneously solving problems in which a response of interest is influenced by several
variables and the objectives is to optimize this response [63].

Figure 8: Flowchart Outlining the Analysis Steps Undertaken

It also has important applications in the design, development and formulation of new
products, as well as in the improvement of existing product designs. The field of response
surface methodology consists of the experimental strategy for exploring the space of the
process or independent variables, empirical statistic modeling to develop an appropri-
ate approximating relationship between the responses and process variables, and opti-
mization methods for finding the levels or values of the process variables that produce
desirable values of the responses. The main advantage of RSM is the reduced number of
experimental runs needed to provide sufficient information for statistically acceptable
results [64].

25
3.6 Factors Affecting the Quality of the Product
Quality of the chalk can be affected by different factors such as particle size, calcinations
temperature, moisture content, calcinations time, moulding time and other minor fac-
tors. However, none of these factors are equally contributes to the quality of the product.
Out of these factors affecting the quality of the product, particle size, calcinations tem-
perature, and moisture content are the most relevant factors due to their significant in-
fluence [59]. Central Composite Design (CCD) was used and the data were analyzed with
Design-Expert 7.0 program. CCD of RSM was used to determine optimum conditions for
testing responses parameters[65]. Therefore, in this work, optimization of process pa-
rameters (PS, CT and MC) for testing the responses (bulk density and breaking strength)
of the product had been carried out and the influence of process variables on these re-
sponses of the product was analyzed.

3.6.1 Experimental Set-up

The setting of the process variables was done based on the chemical proximate compo-
sition of the raw materials, different literatures and preliminary tests. These ranges of
the factors have been selected by practical experience of the process and then conduct-
ing pre-experimentation tests. CCD is well suited for fitting model surface, which usually
works well for process optimization because it includes center and axial points [66]. Cen-
ter points, for which all the factor values are at the zero (or midrange) value. Axial (or star)
points, for which all but one factor are set at zero (midrange) and the other factors are set
at outer (axial) values [67].

Table 12: Coded and Actual levels of the variables for CCD of the RSM
Factors Unit Coded level 1 Level 2 Level 3
symbol (-1) (0) (+1)
Particle Size (m) A 45 70 95
o
Calcinations Temperature C B 135 140 145
Moisture content % C 5 6 7

Face centered composite design (FCCD) for three factors (particle size, calcinations
temperature and moisture content) and three level combinations with total number of
20 runs were used to conduct the study.

Number of factors, f = 3

Run = 2k + 2k + nc = 23 + 2x3 + 6 = 8 + 6 + 6 = 20 and Replicate, r = 3

Number of total experiments = 20 * 3 = 60

The study was conducted to optimize the process variables to produce quality chalk by
varying the process variables of particle size (45, 70, 95m), calcinations temperature
(135, 140, 145o C), and moisture content (5, 6 and 7%). The aim of varying these variables

26
was to get different values of responses (bulk density and breaking strength). The data
obtained from the experimental laboratory was analyzed using the software to determine
the optimum response variables.

Means comparisons was performed using analysis of variance (ANOVA). Finally, the prod-
ucts were selected which gave a better responses and the validation was done on the
selected parameters. Studies were conducted using the RSM in modeling the physical
properties as affected by main variables of individual and their interaction effects. The
independent and dependent variables were fitted to the second order model equation
and examined for the goodness of fit. The behavior of responses variables as a function
of regression explanatory variables were represented by RSM using the following equa-
tion:
Yi = o + 1 A + 2 B + 3 C + 12 AB + 13 AC + 23 BC + 11 A2 + 22 B 2 + 33 C 2 +
...................................................................(4)
Where: Yi - the response function (i stands for bulk density and breaking strength);
o - constant; ij - regression coefficients (i = 1,2,3 and j = 1,2,3,);
A - Particle size; B - Calcinations temperature; C - Moisture content and; - Random error

Table 13: Experimental design setup using design expert CCD

Run A:Particle Size B:Calcinations Temp. C:Moisture Content
1 45 140 6
2 70 140 6
3 95 135 7
4 70 135 6
5 70 145 7
6 70 145 6
7 95 145 7
8 70 140 7
9 45 145 5
10 70 145 5
11 95 135 5
12 95 145 5
13 95 140 6
14 70 140 5
15 45 145 7
16 45 140 5
17 95 140 7
18 95 145 6
19 45 135 7
20 45 135 5

The resulting data for optimization of quality chalk production from gypsum and
the effect of three operating variables were analyzed to generate significant effects with
two responses. Numerical optimization techniques of the Design-Expert softwares were
used for simultaneous optimization of the multiple responses [68].

27
4 RESULTS AND DISCUSSION

4.1 Characterization of the Raw Materials

4.1.1 Physical Characterization

The raw material collected was first characterized physically in such a way that visual
observations, touching and trying to break it. The physical characterization of the raw
materials was as in Table 14.
Table 14: Physical characterization of the raw materials
Properties Color Density Breakage
Type/amounts White 2.3 g/cm3 1.5 Mohs scale

4.1.2 Chemical Characterization

The samples were tested at the central laboratory of the Geological Surveys of Ethiopia
(GSE).
a. Kentry chemical analyses of gypsum: To determine the quality of the potential target,
the samples were tested for CaO, SO3 and H2 O and the following average values were
obtained as in Table 15:
Table 15: Compositional analysis of Kentry gypsum
Compounds CaO(%) SO3 (%) H2 O(%) Others (%) Total (%)
Compositions 37.40 49.98 11.03 1.59 100
Literature Review 32.6 46.5 20.9 - 100

This implies gypsum contains higher composition of SO3 and lower composition of
water. Therefore, these values are within acceptable limit to exploit the occurrence as a
raw material for POP and chalk. Moreover, the average compositional analysis results of
the crushed samples compositions were tested and the results are in Table 16.

Table 16: Compositional analysis of Kentry gypsum after crushed

Compounds CaO(%) SO3 (%) H2 O(%) LOI (CO2 ) (%) Others (%) Total (%)
Compositions 38.47 44.18 7.96 6.52 2.87 100
Literature Review 32.6 46.5 20.9 - - 100

As it can seen from the average values the water content tends to be lower and LOI
tends to be relatively higher, which indicates that the crushed samples contain limestone
fragments (impurities) that consequently increase in LOI and reduce in water content.
b. Filiklik (Blue Nile Gorge) chemical analyses of gypsum: The compositional analyses
of this gypsum are the following:
Therefore, the gypsum occurrence is within acceptable limit to exploit as a raw mate-
rial for POP and chalk.
c. Yogef chemical analyses of gypsum: The compositional analyses are described for
both lower and upper gypsum:

28
 Table 17: Compositional analysis of Filiklik gypsum
Compounds CaO(%) SO3 (%) H2 O(%) Others (%) Total (%)
Compositions 38.23 50.43 10.62 0.72 100
Literature Review 32.6 46.5 20.9 - 100

Table 18: Compositional analysis of lower and upper Yogef gypsum

Compounds(%) CaO SO3 H2 O LOI SiO2 F e2 O3 AlO3 Others Total
Lower gypsum bed 30.75 44.57 16.87 5.27 0.92 0.12 0.11 1.39 100
Upper gypsum bed 30.99 45.61 18.67 3.70 0.79 0.09 0.11 0.04 100
Literature Review 32.6 46.5 20.9 - - - - - 100

Therefore, the gypsum occurrence is within acceptable limit to exploit as a raw mate-
rial for POP and chalk. The comparisons of all the above tables in terms of their distances
from Addis Ababa and the resources capacity were summarized in the Table 19 below.
From this table the gypsum quarried from Kentry was selected in terms of distances from
Addis Ababa and resources capacity. The Yogef (Upper gypsum bed) contains water con-
tent than the others whereas Filiklik gypsum contains more percentages of CaO and SO3
than the rest.

Table 19: Comparison of compositional analyses for the raw materials

Description Dist.from A.A CaO(%) SO3 (%) H2 O(%) Access Resources(Tons)
Kentry 63km 37.40 49.98 11.03 Good Up to 106
Filiklik 202km 38.23 50.43 10.62 Good (3-5)*105
Yogef (LGB) 158km 30.75 44.57 16.87 Good 218,350
Yogef (UGB) 158km 30.99 45.61 18.67 Good 796,068
Literature Review - 32.6 46.5 20.9 - -

4.2 Statistical Results

Particle size (A), calcinations temperature(B) and moisture content(C) were chosen as
the independent variables while the bulk density (Y1 ) and breaking strength (Y2 ) were se-
lected as the response (dependent variable) in the present study. According to the CCD,
a series of experiments was conducted for exploring different combination parameters
and for evaluating the combined effects of these factors.

The aim of present work was to achieve optimized formulations for quality chalk by
determining the effects of important factors and their interactions on physicochemical
properties. Meanwhile the influence of different factors had been evaluated by making
changes in these factors and three of the most significant factors had been chosen as the
independent variables. The experiments were conducted and the results were collected
according to the experimental design output of the software to minimize equipment and
human error.

29
4.2.1 Optimization using Desirability

In this study, CCD was used for response surface optimization with three process vari-
ables (particle size, calcinations temperature and moisture content) at three levels. De-
signs using CCD are usually very efficient in terms of the number of required runs and
therefore are less expensive to run compared to general factorial design.

In most RSM problems, the form of the relationship between the response and the in-
dependent variables is unknown. Thus, the first step in RSM is to find a suitable ap-
proximation for the true functional relationship between dependent and independent
variables. Usually, a low-order polynomial in some region of the independent variables
is employed. If the response is well modeled by a linear function of the independent vari-
ables then the approximating functions is the first order model. If there is curvature in
the system, then a polynomial of higher degree must be used, such as the second-order
model.

RSM is a sequential procedure. Our objective here is to lead our experiment rapidly
and efficiently along a path of improvement toward the general vicinity of the optimum.
Once the region of the optimum has been found, a more elaborate model, such as the
second-order model may be employed, and an analysis may be performed to locate the
optimum. The eventual objective of RSM is to determine the optimum operating con-
ditions for the system or to determine a region of the factor space in which operating
requirements are satisfied.

A 20 runs with three replicate and a total of 60 experiments were conducted for optimiza-
tion of process parameters. The laboratory results of the experiment have been collected
depending on the run order recommended by the Design-Expert software (version 7.0,
Stat Ease) software and the average result of the three replicate was taken as one run and
tabulated in the Table 20.

Analysis of variance was employed to determine the significance of the models. The test
for the significance of the regression models, the test for significance on individual model
coefficients, F-test and the lack-of-fit test were performed using the same statistical soft-
ware package to obtain the best fit. The larger the value of F and the smaller the value of
p, the more significant is the corresponding coefficient term [71]. The coefficient of de-
termination (R2 ) is defined as ratio of sum of squares due to regression to the total sum
of squares and is interpreted as the proportion of the variability in the data explained by
the ANOVA. The words lack of fit refers to the fact that the simple linear regression model
may not adequately fit the data [72]. Prediction error sum of squares (PRESS) is a mea-
sure of how well the model for the experiment is likely to predict the responses in a new
experiment. Smaller values of PRESS are desirable[73]. Verification of optimized param-

30
eters and predicted values were done in triplicate to confirm the validity of the models.

The results were analyzed by applying the coefficient of determination (R2 ), analysis of
variance (ANOVA) and response plots. The response surfaces help to understand the ef-
fect of process variables and parameters up on the responses and direction the response
in which it increases or decreases. The actual experimental values were quantitatively
compared with the predicted values to compute the prediction error (%). Linear corre-
lation between the actual and predicted values of each response was evaluated from the
error (%) to obtain the R2 values for optimum model validation[68].

The optimized formulation was selected making use of desirability functions. Each
Table 20: Statistical results for actual and experimental
Run A:PS B:CT C:MC Bulk Density(g/cm3 ) Breaking Strength (N/cm)
1 45 140 6 1.206 13.3
2 70 140 6 1.150 14.0
3 95 135 7 1.104 12.0
4 70 135 6 1.166 13.8
5 70 145 7 1.125 11.8
6 70 145 6 1.135 14.3
7 95 145 7 1.064 12.6
8 70 140 7 1.145 11.5
9 45 145 5 1.193 15.9
10 70 145 5 1.140 16.6
11 95 135 5 1.120 17.0
12 95 145 5 1.084 17.5
13 95 140 6 1.093 14.9
14 70 140 5 1.154 16.4
15 45 145 7 1.181 10.8
16 45 140 5 1.210 15.7
17 95 140 7 1.088 12.4
18 95 145 6 1.075 15.2
19 45 135 7 1.214 10.2
20 45 135 5 1.225 15.5

response is associated with its own partial desirability function. If the value of the re-
sponse is optimum, its desirability equals 1, and if it is totally unacceptable, its value is
zero[69]. Thus the desirability for each response can be calculated at a given point in
the experimental domain. The optimum is the point with the highest value for the de-
sirability. Various 3-D response surface graphs and contour plots were studied over the
entire experimental region, to select optimum checkpoint formulations for validation of
the experimental domain and polynomial equation.

From over view of the results in Table 20, the maximum bulk density (1.225 g/cm3 ) has
been obtained at PS (45m), CT (135o C) and MC (5%) whereas the minimum bulk density
(1.064 g/cm3 ) has been observed at PS (95m), CT (145o C) and MC (7%). Similarly, the
maximum breaking strength (17.50 N/cm) has been obtained at PS (95m), CT (145o C)

31
and MC (5%) whereas the minimum breaking strength (10.20 N/cm) has been observed
at PS (45m), CT (135o C) and (MC 7%). All experiments were carried out in a random-
ized order to minimize the effect of unexpected variability in the observed response due
to extraneous factors.

The numerical optimization of the software has been chosen in order to find the specific
point that maximizes the desirability function. The desired goal was selected by adjust-
ing the weight or importance that might alter the characteristics of a goal. The goal fields
for responses have five options: none, maximum, minimum, target and within range and
given Table 21.

Table 21: Optimization criteria used in this study

Name Unit Goal Lower Limit Upper Limit
Particle Size (m) in range 45 95
Calcinations Temperature o C minimize 135 145
Moisture content % in range 5 7
3
Bulk Density g/cm target 1.064 1.225
Breaking Strength N/cm target 10.2 17.5

Model selection for further analysis: Two different tests, namely, sequential model
sum of squares and model summary statistic were performed to check the adequacy of
the models generated from the obtained data. The result from the sequential model se-
lects the highest order polynomial where the additional terms are significant and the
model is not aliased. Model summary statistics output showed that the values for the
R2 and adjusted R2 were the highest compared with the other models while the cubic
model was disregarded as it is aliased [70]. The fitness of the models was determined
by R2 and adjusted R2 such that the higher value of R2 the better the model. Therefore,
the two models suggested that 2FI for bulk density and quadratic model for breaking
strength provided an excellent explanation for the relationship between the indepen-
dent variables and the corresponding response. The results from these two models tests
indicated that these models could be used to navigate the design space and provide a
good description of the experimental data and for this reason, it was selected as the most
appropriate model for further analysis.

4.2.2 Development of Regression Model Equation

The coefficients of 2FI and quadratic equations which included only statistically signif-
icant (p<0.05) coefficients for each response were generated as in Appendix B (b and c).
The equation 5 and 6 were formed from that coefficient and a positive coefficient indi-
cates that response is favored, while a negative value indicates an inverse relationship
between the factor and the response.

The second order equations predicting the optimal point was achieved according to the

32
central composite experimental design and input variables, and the empirical relation-
ship between the response and the independent variables in the coded units based on
the experimental results was given below. Coded factors indicate when the minimum,
mid and maximum values of the factors are represented by -1, 0 and +1, respectively in-
stead of actual values. The output response surface bulk density and breaking strength
are a function of the process parameters such as a particle (A), calcinations temperature
(B) and moisture content (C).
I. Bulk Density
pper gypsum bed Density = Y1 = [+1.15 - 0.056*A - 0.017*B + 7.000E-003*C - 1.377E-003
*A*B - 1.695E003*A*C] ...........................................................(5)
From equation (5) the coefficients of A and B were negative whereas the coefficient of
C is positive. Therefore, particle size and calcinations temperature was negatively affect
the bulk density whereas moisture content was positively affect bulk density. The coeffi-
cients of the two factors interaction also negative showing that they have negative effect
on the response.
II. Breaking Strength
Breaking Strength = Y2 = [+14.06 + 0.84*A + 0.26*B - 2.51*C + 0.071*A*C + 0.051*B*C -
0.12*C 2 ] .....................................................(6)
From equation (6) the coefficients of A and B were positive, whereas the coefficient of
C was negative. Therefore, breaking strength was positively affected by particle size and
calcinations temperature, and negatively affected by moisture content. The coefficients
of the two factors interaction (AC, BC) were positive and the quadratic C 2 was negative
effect on the breaking strength.

Confirmation Experiments
The data were also analyzed to check the correlation between the experimental and pre-
dicted values for the responses as shown in Table 20. The experimental values were the
measured response data for the runs designed by the Central composite model, while
the predicted values were obtained by calculation from the 2FI and quadratic equation
for bulk density and breaking strength respectively. The results show that experimental
data and data obtained by regression equation closely correlate with each other, which
validate the regression equations developed.

4.3 Data Analysis of Process Parameters

Data obtained from the experiment were analyzed with the help of software for optimiza-
tion of processing and operating parameters with respect to the responses of the quality
chalk. Multiple regressions analysis and ANOVA were conducted for fitting the model
and to examine statistical significance of the model terms for each response. The statis-
tical analysis of data and three-dimensional plotting were performed using the software.
The adequacies of the models were determined using model analysis, lack of fit test, R2 ,

33
Adjusted R2 , Precision R2 , Adjusted precision and F-test analysis as outlined.

4.3.1 Data Analysis for Bulk Density

From the ANOVA table 22, the data was tested by different values. The Model F-value
(3107.95) with low probability value (p < 0.0001) statistically signifies the model. There
is only a 0.01% chance that a "Model F-Value" this large could occur due to noise. The
linear terms of particle size, calcinations temperature and moisture content, and the in-
teraction between particle size and calcinations temperature; particle size and moisture
content were significant at p < 0.0001 level and all the quadratic terms were not. Values
of "Prob > F" less than 0.05 indicate model terms are significant. In this case A, B, C, AB
and AC are significant model terms. Values greater than 0.10 indicate the model terms
are not significant.

Table 22: Analysis of variance table for improved model for Bulk Density
Source Sum of squares Df Mean square F-value P-value Remark
Model 0.048 5 7.934103 3107.95 <0.0001 significant
A 0.039 1 0.039 12793.29 <0.0001
B 3.622103 1 3.622103 1201.90 <0.0001
C 6.707104 1 6.344104 210.52 <0.0001
AB 1.674105 1 1.656105 5.54 0.0348
AC 2.814105 1 2.269105 9.34 0.0090
Residual 3.917105 14 2.621106
Lack of fit 2.265104 2 1.887105 0.27 0.8907 not significant
Pure error 1.805104 4 1.805104
Cor Total 48.6 19
R2 = 0.9991; Pred.R2 = 0.9980; Adj.R2 = 0.9988; and Adeq.Precision = 166.039

If there are many insignificant model terms (not counting those required to support
hierarchy), model reduction may improve the model. An insignificant lack of fit 0.27 im-
plies that the model was robust enough to explain the effects of the three parameters
on bulk density. Model fitting with the help of Design-Expert software suggested that a
two-factor interactions model provided the best fit, and the model was found to have in-
significant lack of fit. This was desirable as we want a model that fit.
By selecting the step-wise regression method, which eliminates the insignificant model
terms automatically, Tables 26 also show the other adequacy measures R2 , adjusted R2
and predicted R2 . The fit of the model was checked by the coefficient of determination
R2 for bulk density was calculated 0.9991, which is very close to 1, indicating that 99.91%
of variability in the response could be explained by the model and only 0.09% were not
explained by the model. CV (Coefficient of Variation) value to check the reliability and
precision of the model obtained from the model was 0.15%.

In this case, the values of PRESS are considerably smaller. The Predicted R2 of 0.9980
is in reasonable agreement with the Adjusted R2 of 0.9988 with the difference of 0.08%
that signifies a good adjustment of the theoretical values to the experimental data by the

34
model. Adequate Precision measures the signal to noise ratio and a ratio greater than 4 is
desirable. The ratio of 166.039 was much greater than 4 that indicates an adequate signal
and the model can be used to navigate the design space.

4.3.2 Data Analysis for Breaking Strength

The same procedure has been applied on this response as that of bulk density. By se-
lecting the backward elimination procedure to automatically reduce the terms that were
not significant, the resulting ANOVA table for the reduced quadratic model for breaking
strength was displayed. The adequacy of the developed models was tested at 95 % con-
fidence interval and the results of the linear and quadratic order response surface model
fitting in the form of ANOVA was given in Table 23. The ANOVA results (Table 23) indi-
cated that the model F-value of 4868.10 was greater than F0.05 = 2.52, implying that most
of the variation in the response could be explained by the regression equation and that
the model was significant. Furthermore, the probability p<0.0001 also suggested that the
model was significant. There is only a 0.01% chance that a Model F-Value this large could
occur due to noise. Values of Prob > F less than 0.05 indicate model terms are also signif-
icant. The "Lack of Fit F-value" of 0.36 implies the Lack of Fit is not significant relative to
the pure error. Non-significant lack of fit is good since we want the model to fit. In this
case A, B, C, AC, BC and C 2 are significant model terms. Breaking strength was signifi-
cantly affected by linear terms of the parameters at (p < 0.0001); the interaction between
particle size and moisture content, calcinations temperature and moisture content, and
the quadratic of the moisture content with effect of (p<0.005). The lower value of CV
0.39% indicates greater reliability of the experiments performed with smaller values of
PRESS of 0.096.

Table 23: Analysis of variance table for improved model for Breaking Strength
Source Sum of squares Df Mean square F-value P-value Remark
Model 89.54 6 14.92 4868.10 <0.0001 significant
A 8.75 1 8.75 2853.46 <0.0001
B 0.86 1 0.86 279.452 <0.0001
C 83.41 1 83.41 27207.08 <0.0001
AC 0.049 1 0.049 15.94 0.0062
BC 0.025 1 0.025 8.27 0.0203
C2 0.061 1 0.061 19.87 0.0026
Residual 0.040 13 3.066103
Lack of fit 0.59 11 0.045 0.36 0.8799 not significant
Pure error 0.13 5 0.13
Cor Total 89.58 19
R2 = 0.9996; Pred.R2 = 0.9989; Adj.R2 = 0.9993; and Adeq.Precision = 220.081

High multiple correlation coefficient (R2 ) value of 0.9996, which is very close to 1, sig-
nifies a good model explanation where only 0.04% of total variation was not explained by
the model. A reasonable agreement between the Predicted R2 (0.9989) and Adjusted R2
(0.9993) with 0.04% difference indicates a good correlation between the observed and

35
predicted values. Adequate Precision measures the signal-to-noise ratio, with a ratio
greater than 4 considered as desirable. The Adequate Precision ratio of 220.081 obtained
in this study indicates an adequate signal and this model can be used to navigate the
design space. These insignificant model terms (not counting those required to support
hierarchy) should be removed from the model itself and make it into an improved model.

4.3.3 Diagnostic test

Usually, it is necessary to check the fitted model to ensure that it provide an adequate ap-
proximation to the real system. Unless the model showed an adequate fit, proceedings
with the investigation and optimization of the fitted response surface likely give poor or
misleading results. The residuals from the least squares fit played an important role in
judging model adequacy. The quality of the model developed could be evaluated from
their coefficients of correlation. By constructing a normal probability plot of the residu-
als, a check was made for the normality assumption, was given (Fig. 10). All diagnostic

Figure 9: Plots of Residuals for a) bulk density b) breaking strength

Figure 10: Plot of the actual and predicted values for a) bulk density b) breaking strength

plots were also tested for both responses for adequacy of the models (normal plot of
residuals, residuals versus predicted value, residuals versus factor, box Cox plot, studen-
tized residuals, leverage, etc.). As both models showed a satisfactory fit, normal proba-

36
bility plot of the residuals were generated to check the normality of the residuals. The
residuals were studentized and values which were greater than +2 and less than -2 were
considered as large. As both models showed a satisfactory fit, normal probability plot of
the residuals were generated to check the normality of the residuals (Figure 9). Obtaining
a smaller residual value is preferred as this shows the degree of deviancy from predicted
model. It is clear from figure that the residuals followed normal distribution well as ma-
jority of the data points followed the fitted line closely with no reasonable outliers.

The actual and predicted values for both responses were given in Figure 10. From the
figures the predicted data of the response from the empirical model is in good agree-
ment with the observed ones in the range of the operating variables. It shows how pre-
cisely bulk density and breaking strength were modeled because the entire points lineup
nicely. A line of unit slope, i.e. the line of perfect fit with points corresponding to zero er-
ror between predicted and actual values. This plot therefore visualizes the performance
of the correlation in an obvious way[60].

Correlation Matrix for Optimization

The correlation matrix is one of the most common and useful statistics. The correlation
coefficient measures the strength of linear relationships between the variables [72]. The
correlation coefficient is always between -1 and +1. The closer the correlation to +/-1,
the closer to perfect linear relationships[67]. From Appendix B (d) almost all, the factor-
to-factor correlation is zero. For the factor -to-factor correlation of diagonal values close
zero are better which is satisfied in this case.

4.3.4 Effect of Processes Parameters on the Responses

The detailed main and interaction effects for both the responses are discussed in the fol-
lowing sections. It should be noted that if a particular parameter does not influence the
responses during the course of evaluation, it gets eliminated.

Perturbation Plot
Perturbation plot shows how a function of a certain factor responded as the level of that
factor changes, when the other factors are fixed at their optimum levels. A steep slope or
curvature in the plots indicates the sensitivity of the response factor. Perturbation plot
for bulk density and breaking strength (Appendix C (a)) are used to assess the effect of
each factor on the responses. For the bulk density, response increment was observed as
particle size and calcinations temperature were decreased; but moisture content plays
minimal influence on the response. For breaking strength, by comparing the slope of ev-
ery factor, the increment of the response was observed as particle size and calcinations
temperature factors were increased, and the moisture content decreased.

37
Influence of Individual Effect
The individual effect of particle size, calcinations temperature and moisture content
towards bulk density and breaking strength were plotted in the Appendix B (b and c)
respectively. The bulk density was decreased from 1.195g/cm3 to 1.101g/cm3 with the
strictly increasing particle size from 45m to 95m. It also decreased from 1.165g/cm3
to 1.125g/cm3 with smoothly increasing of calcinations temperature from 135o C to 145o C
and decreasing of moisture content from 7% to 5%. This is due to the negative coefficient
of two-factor interaction model as shown in equation 5. It also indicates that the experi-
mental value must consider running effect of particle size and calcinations temperature
at a higher level to minimize the bulk density. At the same time, maximum bulk density
was found from the lower value of particle size and calcinations temperature and higher
value of moisture content. Similarly, breaking strength was increased from 13N/cm to
15N/cm with increasing of particle size from 45m to 95m and 13.8N/cm to 14N/cm
with smoothly increasing of calcinations temperature from 135o C to 145o C and it was
decreased from 16N/cm to 11N/cm with strictly increasing moisture content from 5% to
7%. This due to the positive coefficient of two factor interactions and negative coeffi-
cient of quadratic moisture content in the equation 6. Therefore, the maximum breaking
strength was obtained at higher value of particle size and calcinations temperature, and
lower value of moisture content.

Influence of Interaction Effect

The interaction effects of variables on responses were studied by plotting two factor in-
teractions (Appendix C(d and e)), Contour plot (Appendix C (f and g)) and 3-D surface
curves (Figures 12 and 14) against any two independent variables and keeping another
variable at its central (0) level. The 3-D curves of the calculated responses plots from
the interactions between the variables are shown in Figure 12(a - c), using the statistical
software. The corresponding contour plots (Appendix C (f and g)), represented by the
projection of the response surfaces in the x-y plane, provide a straightforward determi-
nation of the effects of the independent variables on the dependent variable.

I. Bulk density
Interaction between process variables can affect the bulk density and these effects have
been seen statistically and graphically. a. Effect of Particle Size - Calcinations Tempera-
ture (AB) on Bulk Density
AB = 2/4[1.10 + 1.23 + 1.07 + 1.19 - 1.18 - 1.08 - 1.21 - 1.12] = 0.0012
b. Particle Size - Moisture Content (AC) Effect
AC = 2/4[1.23 + 1.21 + 1.08 + 1.07 - 1.18 - 1.19 - 1.10 - 1.12] = 0.0024
c. Calcinations Temperature - Moisture Content (BC) Effect
BC = 2/4[1.23 + 1.12 + 1.18 + 1.07 - 1.19 - 1.08 - 1.21 - 1.10] = 0
These results show that the interactions of particle size - calcinations temperature and
particle size-moisture content have minimum effect on bulk density whereas the inter-

38
Figure 11: Cubic representation of interaction effects of the three factors on bulk density

action of calcinations temperature - moisture content has not. This was shown graphi-
cally in Appendix C (d). From the graph, it was seen that the lines are almost parallel that
shows there was no significant interaction effect between the two factors.

Response Surface for Bulk Density

Figure 12(a-c) shows the interactions effects of particle size, calcinations temperature
and moisture content on the response variable of bulk density. The response surface
plots in three figures were both part of a diagonal, exhibiting a minimum and maximum
ridge, respectively, in the investigated domain. In each response surface, the optimum
values of variables could be analyzed by the saddle point or by determining the maxima
formed by the x- and y-coordinates.

Figure 12: Response surface plots for bulk density as a function of three factors

Figure 12a depicts the interaction effect of particle size and calcinations temperature on
bulk density at constant moisture content of 6%. It has been seen that, at given constant
moisture content, bulk density uptake increased with decreasing calcinations temper-
ature smoothly and particle size strictly. However, increasing calcinations temperature
and particle size decreases bulk density.

39
Figure 12b depicts the interaction effect of particle size and moisture content on bulk
density at constant calcinations temperature of 140o C. When size of the particle de-
creased and the moisture content increased, the bulk density was increased. However,
increasing particle size and decreasing moisture content decreases bulk density.

Figure 12c depicts the interaction effect of calcinations temperature and moisture con-
tent on bulk density at constant particle size of 70m. As calcinations temperature in-
creased and moisture content decreased, the bulk density was decreased. However, de-
creasing calcinations temperature and increasing moisture content increase bulk den-
sity.

Generally, it was understood from these three figures that when the size of the particle is
small, minimum temperature was needed to evaporate moisture content. As maximum
percentage of moisture content was evaporated from the sample, the product become
dry. When the size of the particle is large, it needs maximum temperature to evaporate
the moisture content it has. As maximum percentage of moisture content was left in the
particle, the product become humid. This is the reason why it was wanted to take the
optimum values of these variables from the range to get the targeted bulk density.

II. Breaking strength

Interaction between process variables can affect the breaking strength and these effects
have been seen statistically and graphically.

Figure 13: Cubic representation of interaction effects of the three factors on breaking
strength

a. Particle Size - Calcinations Temperature (AB) Effect

AB = 2/[15.47 + 12.03 + 12.66 + 15.90 - 10.84 - 17.43 - 10.22 - 17.01] = 0
b. Particle Size - Moisture Content (AC) Effect
AC = 2/4[15.47 + 10.22 + 17.43 + 12.66 - 17.01 - 12.03 - 15.90 - 10.84] = 0.007
c. Calcinations Temperature - Moisture Content (BC) Effect
BC = 2/4[15.47 + 17.01+ 10.84 + 12.66 - 10.22 - 12.03 - 15.90 - 17.43] = 0.05
These results show that the interactions of particle size - calcinations temperature has no

40
effect on the breaking strength whereas the interactions particle size - moisture content
and calcinations temperature - moisture content have minimum effects on the response.
This is shown graphically in Appendix C (e). From the graph, it was has been seen that
the lines are almost parallel that shows there is no significant interaction effect between
the two factors.

Response Surface for Breaking Strength

Figure 14(a-c) show interaction effects of particle size, calcinations temperature and mois-
ture content on the response variable of breaking strength. The response surface plots
in figure 14a was part of rectangle and that of figures 14b and 14c were part of a diagonal
exhibiting a minimum and maximum in the investigated domain. In each response sur-
face, the saddle could analyze the optimum values of variables.

Figure 14a depicts the interaction effect of particle size and calcinations temperature on

Figure 14: Response surface plots for breaking strength as a function of the three factors

breaking strength at constant moisture content of 6%. As particle size and calcinations
temperature increased, breaking strength also increased. However, decreasing calcina-
tions temperature and particle size decrease breaking strength.

Figure 14b depicts the interaction effect of particle size and moisture content on break-
ing strength at constant calcinations temperature of 140o C. As the size of the particle in-
creased and moisture content decreased, the breaking strength was increased. However,
decreasing particle size and increasing moisture content decrease breaking strength.

Figure 14c depicts the interaction effect of calcinations temperature and moisture con-
tent on breaking strength at constant of particle size 70m. When calcinations temper-
ature increased and moisture content decreased, the breaking strength also increased.

41
However, decreasing calcinations temperature and increasing moisture content decrease
breaking strength.

It was understood from these figures that; when there is much moisture content in the
sample, the product become soft and it can be broken easily. But as the moisture content
was minimized in the sample, the product become hard, and the chalk has a sound of
disturbance when use with it.

Similarly, as the size of the particle was reduced to very small diameter, the product can
break easily. But when the diameter was increased, the final product may not break as
such. This is the reason why it was wanted to take the optimum values of these variables
from the range to get the targeted breaking strength.

4.3.5 Optimization of the Process Parameters

The primary objective of the present study was to find the optimum process parameters
to get optimum responses of good quality chalk. Numerical optimization step in CCD
was used to predict the optimum values of bulk density and breaking strength by the
adjusted model. The goals for variables of particle size and moisture content were set as
in range whereas calcinations temperature was minimize. The goals for the responses
(bulk density and breaking strength) were set as target because the optimum values
of bulk density and breaking strength were neither at maximum point nor at minimum
point. Desirability function was used to identify the optimum levels of factors and to get
maximum desirable response. The individual desirability and the combined desirability
of both responses were reported in table below via numerical optimization.

Table 24: Optimum solutions obtained depending on the desirability

S.N Particle Calcination Moisture Bulk Breaking Desirability
Size Temperature Content Density Strength

1 85.55 137.00 6.25 1.1445 13.85 0.998

2 80.35 139.55 6.11 1.1442 13.85 0.992
3 80.35 142.64 6.11 1.1452 13.85 0.948
4 80.62 139.25 5.98 1.1441 14.25 0.925
5 80.81 138.06 6.57 1.431 13.04 0.915

The standard ranges for bulk density and breaking strength are between 1.112 - 1.201
g/cm3 and 10 - 20N/cm respectively[74][75]. The values, which are out of these ranges,
are not considered in the optimization domain. The values that are in these ranges are
identified by their desirability, the value that has maximum desirability was taken as an
optimum value. Therefore, as it can be seen from Table 24 below, a number of solutions
was produced by the software and ranked according to their desirability. The optimized

42
batch was selected with maximum combined desirability value i.e. 0.998 using the soft-
ware.

The solutions with the highest desirability were chosen and the optimum values were
1.1445g/cm3 and 13.85N/cm for bulk density and breaking strength respectively at 85.55m
particle size, 137o C calcinations temperature and 6.25% moisture content as optimum
value of process parameters. The experimental values of the response variables obtained
from the optimized formulations were close and in linear with the predicted values.

4.3.6 Validation of Optimum Results

An experiment was set up to validate the optimized condition. As shown in Table 24, the
experimental data were in good agreement with the predicted values for bulk density and
breaking strength. Relative error between predicted and experimental values fell at 0.39%
and 1.21% for bulk density and breaking strength respectively. The verification value
for responses obtained is within 99% of predicted values which clearly showed that the
model fitted the experimental data very well and therefore optimized efficiently within
the specified range of process parameters. The validation results demonstrated that the
models developed are quite accurate as the percentages of error in prediction were in a
good agreement. Thus, the low magnitude of error in this study improves the significant
analytical ability of the model.

Table 25: Validation test results

o
PS(m) CT( C) MC(%) BD(g/cm3 ) BS(N/cm)
85.55 137 6.25 Predicted 1.1445 13.85
Experimental Validated 1.1418 14.02
Error % 0.39 1.21

Once it was understood that the optimum process parameters were obtained from
the experimental result, it was compared with practical chalk factory in Ethiopia as in
Table 26. From this table there was a difference between these results and that of the
practical one. This is the result of this thesis, which found the optimum parameters that
improve the quality of the existing one. Therefore, the quality of chalk produced from
the optimum parameters was strictly different from existing. The comparison of the op-
timum values of the present thesis with the values of literature review was tabulated in
Table 26.

Table 26: The comparison of this result with the literature review
PS(m) CT(o C) MC(%) BD(g/cm3 ) BS(N/cm)
This thesis result 85.55 137 6.25 1.1445 13.85
Literature review 90 135 7 1.14 14.02

As a result of this paper, the size of particle was reduced from 90m to 85.5m, calci-
nations temperature was increased from 135o C to 137o C and the moisture content was

43
reduced from 7% to 6.25%. Because of changing these parameters, the responses also
changed as breaking strength of the chalk decreased from 14N/cm to 13.85N/cm and the
bulk density was increased from 1.14g/cm3 to 1.1445g/cm3 .

Changing these responses eliminated the emits a shrill, piercing and scratching sound
when applied on the blackboard. It also improved the problem of the dryness and diffi-
culties of using chalk. It eliminated the fragmentizes and turns to dust or powder. It was
easily wipe off from the blackboard and broken pieces were not found in the package.

44
5 FEASIBILITY STUDY OF IMPROVED QUALITY CHALK

5.1 Product Description

Chalk sticks are used in all schools and colleges everywhere. It has an indispensable role
in the teaching and learning process being the medium through which the knowledge of
the teacher is transferred to the students. It is a substance used for drawing and writing
on rough surfaces as it readily crumbles leaving particles that stick loosely to these sur-
faces. Chalk also called blackboard chalk often supplied in sticks of about 80mm long
is made from calcium sulphate dihydrate [44]. Ethiopia has nine region with two fed-
eral city totally eleven regions. But there is no chalk industry in any region except Addis
Ababa. The other ten regions have transported chalk sticks from Addis Ababa. Chalk
sticks are made mainly from gypsum, which is found in the many of the regions, and
there is every economic reason for producing chalk sticks [45].

The demand for this product is expected to increase because there is high expansion of
educational institution throughout the country. The consumption of chalk sticks will in-
crease as the number of students and schools increase. The main raw material for chalk
sticks is plaster of Paris or calcium hemi-hydrate, which is obtained by calcinating gyp-
sum. Gypsum is found in many parts of the region in abundant quantity.

Demand Projection: The future demand for chalk depends on a number of interrelated
factors.

Table 27: Demand and supply of chalk in Ethiopia (2000 - 2013)

Year Demand (1000kg) Supply (1000kg)
2000 375.8 278.3
2001 412.6 298.0
2002 460.2 377.7
2003 473.5 380.4
2004 490.0 392.0
2005 514.5 409.5
2006 540.4 411.6
2007 567.0 413.7
2008 595.7 415.1
2009 637.0 420.0
2010 681.8 424.2
2011 750.4 435.4
2012 825.3 451.5
2013 907.9 466.2

Source: FRDE Ministry of Education

45
 These factors that are critical in determining the volume and trend of demand for
chalk include:

The overall economic development level and growth trend of the country;

The performance and expansion of the education sector;

Education budget and expenditure;

Government policies on education; and

Size of the population in general and the school age population in particular.

As it can be seen from Table 27, the demand of chalk and the supply wenclusion re far
apart in terms of quantity. As the number of students increased from year to year rapidly
in the country, the demand of chalk is increasing but the supply of chalk was not increas-
ing with the demand.

Pricing: Currently, chalk factories in Ethiopia and the imported ones sell chalk for
almost the same price, 8 Birr/gross for white chalk and 12 Birr/gross for colored chalk.
Similarly locally produced gypsum sells up to 42.00 Birr per 25kg and imported gypsum
fetches as much as 75 Birr per 25kg.

Plant Capacity: According to the market study and the economic scale of chalk man-
ufacturing, the rated capacity of the plant is proposed to be 3200 gross per day of chalk
of which 60% is white and 40 is colored chalk. The selected production capacity is based
on 300 working days per annum and 16 hours per day by two shifts. The rest of calendar
days are left for cleaning and maintenance

Production Program: The production program is based on the time required for the
adjustment of feedstock, labor and equipment to the technology selected. The plant has
planned to produce 75% of plant capacity during the first year; 85% of plant capacity
during the second year, 100% of plant capacity during the third year and then after.

5.2 Quality Control

Quality is the rated ability of the product to perform its functions. It is the summary
term for the products durability, reliability, precision, ease of operation and repair and
other values of attributes. Quality assurance is an important and necessary function in
any manufacturing company. It provides the necessary know-how to the plants so they
can deliver finished products within the highest standards. The quality control depart-
ment in a plant provides important services by maintaining a high standard of product
quality and by giving proper training to the plant personnel. Todays market is highly

46
competitive. Any company is likely to lose business if it does not possess the capabil-
ity of supplying customers with high-quality product at a competitive price. Therefore,
more than ever before, it is important that the personnel in chalk production plant be
well informed of the techniques of parameter processing, manufacturing, and quality
and cost management [55].

To produce finished products with zero defects, the incoming raw materials must meet
all specifications. Poor quality of gypsum prevents production of the best-quality fin-
ished product at a low cost and increases refining losses. Process operating standards
are critical in order to obtain improved chalk quality with the proper functional proper-
ties and stability.

5.3 Material and Energy Balance

Material and energy balances are the basis of process design. A material balance taken
over the complete process will determine the quantities of raw materials required and
products produced. Balances over individual process units set the process stream flows
and compositions. They are also useful tools for the study of plant operation and trouble
shooting. They can be used to check performance against design; to extend the often-
limited data available from the plant instrumentation; to check instrument calibrations;
and to locate sources of material loss. On the other hand, in process design, energy bal-
ances are made to determine the energy requirements of the process: the heating, cool-
ing and power required. In plant operation, an energy balance (energy audit) on the plant
will show the pattern of energy usage and suggest areas for conservation and savings [73].

In the case of this research, the need to conduct material and energy balances on ma-
jor unit operations that scale up all the parameters used in the laboratory resulted in the
annual production of the plant; in order to design the size of the equipment that helped
in estimating purchased equipment cost. In addition to that, they helped in calculating
the material, auxiliary and utility costs. Generally, they are needed to estimate economic
analysis; profitability and financial feasibility of the processing plant.

5.3.1 Material Balance

Material balance calculations are based on the principles of conservation of mass that
states that matter can be neither created nor destroyed but may go under physical or
chemical change. Material balance can be done on the size reduction process, calcina-
tions, mixer, moulding and drying. General Material balance assumptions:

2 shifts per day

8 working hours per shift

47
 16 working hours per day

300 working days per year

3,200 gross per day or 2,240 kg/day of capacity

3:2 percent ratio of white to colored chalk

The material balance was done by starting from the product gained and gone backward
to determine the amount of raw materials required for processing the plant daily assum-
ing the production capacity 2,240 kg/day.

1. Dryer: Assuming 58% of the total feed is evaporated in dryer.

Wet chalk = vapor + dry chalk

Figure 15: Material balance for dryer

but Vapor = 0.58 * wet chalk

Wet chalk = 0.58 * Wet Chalk + Dry chalk
=> 0.42 Wet chalk = Dry chalk = 2240 kg/day
Wet chalk = 5,333 kg/day and
Vapor = 0.58 * 5333kg/day = 3,093 kg/day

2. Moulding: there is 1% loss in molding due to breakage.

POP Slurry + Wasted Chalk = Wet chalk

Figure 16: Material balance for moulder

but Wasted chalk = 0.01 * POP Slurry

POP Slurry = 0.01 * POP Slurry + Wet chalk
0.99 POP Slurry = Wet chalk = 5,333 kg/day
POP Slurry = 5387 kg/day and

48
Wasted chalk = 0.01 * POP Slurry = 54 kg/day

3. Mixer: In the laboratory result, the amount of clean water to POP is 6/5 in mixer and
loss 0.2%.
POP Powder + Clean water = POP slurry + Wasted POP

Figure 17: Material balance for mixer

But the Clean water/POP Powder = 6/5 = 1.2

=> Clean water = 1.2 * POP Powder and
Wasted POP = 0.002 * (POP Powder + Clean water) = 0.0044 * POP Powder
POP Powder + 1.2 * POP Powder = POP slurry + 0.0044*POP Powder
2.1956 POP Powder = POP slurry = 5,387 kg/day
POP Powder = 2453.54 kg/day and
Clean water = 1.2* 2,453.54 kg/day = 2,944.25 kg/day
Wasted POP = 0.0044 *2,453.54 kg/day = 10.79 kg/day

4. Pulverizing: Considering process loss of 1.1% during pulverizing,

POP = Loss + POP Powder but

Figure 18: Material balance for Pulverizer

Loss = 0.011 * POP

POP = Loss + POP Powder
POP = 0.011 * POP + POP Powder
0.989 POP = POP Powder = 2,453.54 kg/day
POP = 2,480.83 kg/day and Loss = 0.011 * 2,480.83 kg/day = 27.29 kg/day

49
5. Calcinations/Kettle Calciner: According to laboratory result, 18% is losing during cal-
cinations.
Gypsum powder = Water vapor + POP but

Figure 19: Material balance for kettle

Water vapor = 0.18 * Gypsum powder

Gypsum powder = Water vapor + POP
Gypsum powder = 0.18 * Gypsum powder + POP
0.82 Gypsum powder = POP = 2,480.83 kg/day
Gypsum powder = 3025.4 kg/day and Water vapor = 0.18*2,480.83= 446.55 kg/day

6. Grinding Mill: According to laboratory, result 1.5% loss in the grinding mill.
Gypsum from secondary crusher = Loss + Gypsum powder

Figure 20: Material balance for grinding mill

But Loss = 0.015* Gypsum from secondary crusher

Gypsum powder from secondary crusher = 0.015* Gypsum from secondary crusher +
Gypsum powder
0.985Gypsum from secondary crusher = Gypsum powder = 3,025.4 kg/day
Gypsum from secondary crusher = 3,071.48 kg/day and
Loss = 0.015* 3,071.47 = 46 kg/day

7. Secondary Crusher: the process loss of 0.55% during secondary crushing.

Gypsum from jaw crusher = Loss + Gypsum from secondary crusher
But Loss = 0.015* Gypsum from jaw crusher

50
 Figure 21: Material balance for secondary crusher

Gypsum powder from jaw crusher = 0.0055* Gypsum from jaw crusher + Gypsum from
secondary crusher
0.9945 Gypsum from jaw crusher = Gypsum from secondary crusher = 3,071.48 kg/day
Gypsum from jaw crusher = 3,088.47 kg/day and
Loss = 0.0055* 3,071.47 = 17 kg/day

8. Jaw Crusher: According to laboratory result, 0.1% of the raw materials are losing dur-
ing crushing and conveyance to the smaller crushing.
Gypsum rock = Gypsum powder from jaw crusher + Loss

Figure 22: Material balance for jaw crusher

But Loss = 0.001* Gypsum rock

Gypsum rock = Gypsum powder from jaw crusher + 0.001* Gypsum rock
0.999 Gypsum rock = Gypsum powder from jaw crusher = 3,088.47 kg/day
Gypsum rock = 3,091.56 kg/day and
Loss = 0.001* 3,091.56 kg/day = 3.09 kg/day
Therefore, the plant needs the 3,091.56 kg raw materials in a day.

5.3.2 Energy Balance

The general equation for energy balance can be given as:

Accumulation = Energy out - Energy in + Generation - Consumption
Generally, to determine the cooling or heating requirements of any processing industry
simplified equation can be met by ignoring the potential and kinetic energy of the sys-
tem and considering the inlet and out let enthalpy of the system, heat added or removed
from the system. All calculated energy values are the quantity of energy required to run
one batch process[46].

51
Table 30. Thermodynamic properties of compounds

Energy balance can be done on the unit operation: calcinations unit and drying unit.

a. Energy Balance on Kettle Calciner

: Latent heat of evaporation = 2,256 kJ/kg

Figure 23: Energy Balance on Kettle Calciner

QGypsumP owder + Q(ElectricHeating+Steam) = QW aterV apor + QP OP

QGypsumP owder = MGypsumP owder Cp,GypsumP owder (TGypsumP owder - Tr ef )
QGypsumP owder = 3025.38 kg/day * 1.09 kJ/kg.K * (373.15K - 298.15K)
QGypsumP owder = 2.473 X 105 kJ/day
QP OP = MP OP Cp,P OP (TP OP - Tref )
QP OP = 2480.83 kg/day * 1.09 kJ/kg.K * (410.65 K - 298.15K)
QP OP = 3.042 X 105 kJ/day
QW aterV apor = MWv* W aterV apor
QW aterV apor = 446.55 kg/day * 2,256 kJ/kg
QW aterV apor = 10.074 X 105 kJ/day
QGypsumP owder + Q(ElectricHeating+Steam) = QW aterV apor + QP OP
Q(ElectricHeating+Steam) = QW aterV apor + QP OP - QGypsumP owder
Q(ElectricHeating+Steam) = 1,007,416.8 kJ/day + 304,211.78 kJ/day - 247,324.82 kJ/day
Q(ElectricHeating+Steam) = 15.589X 105 kJ/day

b. Energy Balance on Dryer: the wet chalk was dried at temperature of 120o C.
H: Enthalpy (kJ/hr);

Figure 24: Energy Balance on Dryer

52
Q: the total amount of heat to be supplied (kJ/hr);
Mw: Mass flow rate (kg/hr);
Cp: specific heat (kJ/(K.kg)); T: Temperature (K); To = 100K: initial temperature;
Tr = 298K: reference temperature.
H(solid in) + Q = Hv + H(solid out)
11,478 + 53,887 + Q = 388,032 + 14,497
Q = 3.372 x105 kJ/hr

5.4 Design of Equipment

The main objective of this design is to determine the total heat transfer surface area,
diameter, length/height and wall thickness of the equipment and material for construc-
tion.
a) Dimension of the Kettle Calciner
Mass feed rate of CaSO4 .H2 O = 3025.38 kg/hr and density = 2320 kg/m3
Volumetric flow rate of CaSO4 .H2 O = = 1.305 m3 /hr

The time it takes for one batch is 2 hours and 30 minutes

The volume of the kettle = Volumetric flow rate of the CaSO4.H2O * time = 1.305 m3 /hr
*2.5 hrs = 3.7625m3
Assuming 15% safety margin m3 = 3.7625 * 0.15 = 0.564m3
Therefore total volume of the kettle = 3.7625m3 + 0.564 m3 = 4.33m3
From the geometry of material with cylindrical form, the volume = (R2 )h From physical
space of the plant let the height of the kettle be 2.2m. Then, the radius of the kettle can
be calculated as:
4.33m3 = (R2 )h => 4.33m3 = 3.14* 2.2m R2 => R2 = 0.63 => R = 0.81m
Diameter of the mixer, D = 2R = 1.62m
b) Dimension of the Mixer
Mass feed rate of CaSO4 .H2 O = 2453.54 kg/day = 154 kg/hr and density = 2320kg/m3
Mass feed rate of H2 O = 2944.25kg/day = 184 kg/hr and density = 1000kg/m3
Volumetric flow rate of CaSO4 .H2 O = 0.066m3 /hr
Volumetric flow rate of H2 O = 0.184m3 /hr
Volumetric flow rate of the mixture = 0.066 m3 /hr + 0.184m3 /hr = 0.25 m3 /hr
The time it takes in one mixture is 4 minutes
The volume of mixer = Volumetric flow rate of the mixture * mixture time = 0.25m3 /hr *
4minutes = 0.017m3
Assuming 15% safety margin m3 = 0.017 * 0.15 = 0.00255m3
Therefore total volume of the mixer = 0.017 m3 + 0.00255m3 = 0.02m3
From the geometry of material with cylindrical form, the volume = (R2 )h
From physical space of the plant let the height of the mixer be 0.8 m.
Then, the radius of the mixer can be calculated as

53
1.2m3 = (R2 )h => 0.02m3 = 3.14R2 => R2 = 0.008 => R = 0.089m
Diameter of the mixture, D = 2R = 0.18m
c) Dimension of the Moulder
Mass feed rate of slurry = 5387 kg/day = 337kg/hr and density = 2757kg/m3
Volumetric flow rate of slurry = 0.122m3 /hr
The time it takes in one moulding is 15 minutes The volume of the moulder = Volumetric
flow rate of the moulder * mixture time= 0.122m3 /hr * 15 minutes = 0.0306m3
Assuming total 24% safety margin m3 = 0.0306 * 0.24 = 0.00744m3 Therefore total volume
of the moulder = 0.0306m3 + 0.0074m3 = 0.038m3
Volume = (R2 )h and let the height of the moulder be 1m.
Then, the radius of the moulder can be calculated as
0.038 m3 = (R2 )h => 0.038 m2 = 3.14R2 => R2 = 0.013 => R = 0.113m
Diameter of the moulder, D = 2R = 0.226m
From the literature review, diameter and length of piece of chalk is 10mm and 80mm re-
spectively.
Volume of the chalk = 0.00005m3
Number of chalk per hour = 756 pieces/hr = 12096 pieces/day

5.5 Financial Analysis

Experimentally and engineering wise it has been seen that investing chalk production for
the plant is feasible. But, its feasibility should be checked financially. In this section, the
proposed project to be analyzed financially depending on the proposed and designed
chalk production plant according to [74].

5.5.1 Total Capital Investment

The total capital investment (TCI) for the production of blackboard chalk is estimated by
summing up the fixed capital investment (FCI) and working capital. The working capital
(WC) is taken as 15% of the total capital investment (0.15TCI) which is commonly used
[75].
TCI = FCI + WC
a. Machinery and equipment The machinery and equipment cost of the chalk was cal-
culated in table 31 below and the total estimated cost is 6,794,182.75 Birr.
b. Direct and Indirect cost: both the direct and indirect cost of the plant determina-
tion is done based on the ratio of solid-fluid processing plant because of in the produc-
tion of blackboard chalk these processes are included [74].
WC = 15% of TCI = 0.15TCI By substituting this equation in equation above, we get the
following value:
TCI = FCI +WC = FCI + 0.15 TCI => 0.85 TCI = FCI
=>0.85TCI = 17,423,681.78

54
 Table 28: Purchased equipment cost
S.N Description Quantity Unit Price(Birr) Total Cost(Birr)
1 Jaw crusher 1 1,012,888 1,012,888.00
2 Secondary crusher 1 886,198 886,198.00
3 Packing/ bagging 930,576.00
4 Electric control panel 747,114.00
5 Spare parts 410,356.00
6 Weighing scale 2 15,000 30,000.00
7 Moulding 20 45,952 919,042.00
8 Dryer 1 971,811 971,811.00
Contingencies 15% 886,197.75
Total PEC 6,794,182.75

Table 29: Fixed Capital Investment Cost

Cost Category Components Factors Cost (Birr)
Purchased Equipment Cost %PEC 6,794,182.75
Direct Cost (DC) Equipment installation 35 2,377,964.00
Instrumentation and controls 10 679,418.28
Piping (installed) 30 2,038,254.83
Electrical (installed) 10 679,418.28
Buildings (Including services) 20 1,358,836.55
Yard improvements 10 679,418.28
Services facilities (installed) 40 2,717,673.10
Land 4 271,767.31
Total direct cost (DC) 10,802,750.63
Indirect Cost (IC) Engineering and supervision 30 2,038,254.83
Construction expenses 34 2,310,022.14
Total Indirect cost (IC) 4,348,277.00
DC + IC 15,151,027.63
Contractors fee (CF) 5% (DC + IC) 757,551.38
Contingency (C) 10% (DC + IC) 1,515,102.76
FCI DC + IC CF +C 17,423,681.78

=>TCI = 20,498,449.14
WC = 0.15 * 17,423,681.78 = 3,074,767.37

5.5.2 Total Product Cost

The total production cost for the production of board chalk is estimated by summing
up the manufacturing cost and general expenses. The manufacturing costs can be calcu-
lated by adding direct production cost, fixed charge and plant overhead cost and the gen-
eral expenses also calculated by summing up the distribution and marketing expenses,
research and development, financing and gross earnings expenses [76].
Total Product Cost = Manufacturing Cost + General Expenses
Manufacturing Cost = direct production cost + fixed charges + plant overhead costs
General expenses = administrative costs + distribution and selling costs + research and
development costs

55
1. Manufacturing Cost The different type of product cost under manufacturing are cal-
culated as follows:
I. Direct Production Costs (DPC)

Table 30: Raw and auxiliary materials, Utilities cost and Operating Labor Cost
S.N Description Unit Unit Price (Birr) Total Cost (Birr)
A. Raw and Auxiliary Materials
3
1 Gypsum rocks m 43.00 24,295.00
2 Process water m3 3.00 318.00
3 Diesel oil lt 4.50 28,125.00
4 Plastic bag pc 1.30 2,512.90
5 Kerosene lt 3.67 128,101.35
6 Lubricating oil lt 13.75 17,751.25
7 Cola Kg 10.77 3,304.24
8 Carton box pc 0.33 44,384.34
Total 247,792.08
B. Utility Cost
1 Electric power kWh 0.34 36,007.02
2 Water m3 3.00 4,758.00
Total 40,765.02
C. Operating Labor Cost(OLC)
S.N Job Title Persons Monthly(Birr) Annually(Birr)
1 Project manager 1 4,000 48,000
2 Secretary 1 1,300 15,600
3 Documentation clerk 1 600 7,200
4 Accountant and controller 1 1,500 18,000
5 Accounts clerk 1 600 7,200
6 Cashier 1 800 9,600
7 Purchaser 1 800 9,600
8 Store keeper 1 800 9,600
9 Driver 1 600 7,200
10 Production 20 21,700 260,400
11 Guard 2 1,750 21,000
12 Cleaner 1 450 5,400
Total 33 34,900 418,800
Employees Benefit (25% of Basic Salary) 104,700
Total 523,500.00

D. Maintenance and repairs = 4%FCI = 0.04*17,423,681.78 = 696,947.27

E. Laboratory charges = 12% of operating labor = 0.12*523,500 = 62,820.00
F. Operating Supplies =11% of maintenance and repairs = 0.11*696,947.27 = 76,664.20
G. Direct supervisory and clerical labor =15% of operating labor = 0.15*523,500 = 78,525.00
Total direct production cost (DPC) = A + B + C + D + E + F + G
DPC = 247,792.08 + 40,765.02 + 523,500.00 + 696,947.27 + 62,820.00 + 76,664.20 + 78,525.00
DPC = 1,727,013.57 Birr/yr

56
 II. Fixed Charges (FC)
H. Depreciation = 10% FCI = 0.1*17,423,681.78 = 1,742,368.18
I. Capital charge = 1.5% FCI = 0.015*17,423,681.78 = 261,355.23
J. Insurance = 0.5% FCI = 0.005*17,423,681.78 = 87,118.41
Fixed charges = FC = H + I + J = 1,742,368.18 + 261,355.23 + 87,118.41 FC = 2,090,841.82
Birr/yr
III. Plant Overhead Costs (POC)
Plant overhead costs = POC = 10% TPC = 0.1TPC
Manufacturing Cost (MC) = DPC + FC + POC = I + II + III
= 1,727,013.57 + 2,090,841.82 + 0.1 TPC = 3,817,855.39 + 0.1 TPC
1. General Expenses K. Administrative cost = 4% TPC = 0.04TPC
L. Distribution and selling cost = 10% TPC = 0.1TPC
M. Research and Development cost = 5% TPC = 0.05TPC
General Expenses= K + L + M = 0.04 TPC + 0.1TPC + 0.05TPC = 0.19 TPC
Total Production Cost (TPC) = Manufacturing cost + General expenses
TPC = 3,817,855.39 + 0.1 TPC + 0.19 TPC => 0.29 TPC = 3,817,855.39
TPC = 13,165,018.58 Birr/yr

5.5.3 Profitability Measurements

Annual production of chalk = Q = 2240 kg/day x 300 days/yr = 672,000 kg/yr

Totalproductioncost
Unitproductcost = UPC = = 16.59Birr/kg (4)
Annualproduction

Selling price with 25% profit = SP = 0.35*16.59 + 16.59 = 22.4 Birr/kg

Total income per year (TI) = annual production rate * selling price = Q*SP = 672,000 * 22.4
= 15,050,448.00 Birr/yr
a. Gross profit earning (GPE): is the difference between sales and the cost of goods sold
[74].
GPE = Total Income (TI) - Total Product Cost (TPC)
= 15,050,448.00 - 13,165,018.58 = 1,885,429.42 Birr/yr
Net profit earning (NPE): taking the income tax rate of Ethiopia which is 35%,
NPE = GPE - Income tax (0.35*GPE) = GPE (1-0.35) = 0.65GPE
= 0.65 * 1,885,429.42 = 1,225,529.12 Birr/yr
b. Return on investment (ROI): measures the gain or loss generated on an investment
relative to the amount of money invested [74].

NPE 100
ROI = = 6% (5)
TCI

57
c. Payback Period (PBP): It is a period required to recover the original investment outlay
through the accumulated net cash flows earned by the project[75].

FCI
PBP = = 3.6years (6)
NPE + Depreciation

d. Break Even Analysis: The break-even analysis is to determine the point at which sales
revenues equal with the costs of products sold. When sales are below this point, the
plant is making a loss, and at the point where revenues equal to costs, the plant is break-
ing even. The break-even production is the number of units necessary to produce and
sell in order fully to cover the annual fixed costs [76]. It can be computed as:
Total product cost = Total income
To calculate the total product cost and total income, unit product cost of 13.7 birr/kg,
product-selling price of 18.5 birr/kg, were considered. The break-even point was calcu-
lated as [77]:
(Fixed charges + General expenses + Plant overhead costs) + 16.59n = 22.4n
Where n is the number of kg of product produced.
2,090,841.82 + 0.1TPC + 0.19 TPC + 16.59n = 22.4n
2,090,841.82 + 3,817,855.39 = 5.81 n
5,908,697.21 = 5.81n => n = 1,016,987.47 kg

This is the quantity of product at break-even point. It is 52% of the plant capacity. Based
on the preliminary economic evaluation, the suggested project has a return on invest-
ment (ROI) of 6% and payback period of 3.6 years. The break-even production capacity
is at 52%, showing that there is good profit margin. Thus, the suggested project is finan-
cially feasible.

5.6 Plant Location

To select proper locations and sites, certain key requirements or criteria should be set
(i.e. raw material proximity, Infrastructures, product market, human power) that would
allow the assessment of a number of potential locations. The remaining alternatives are
subject to a more in-depth qualitative and quantitative analysis of technical and financial
criteria, including social, environmental and economic aspects of location and site selec-
tion. For gypsum extract producing plant, based on proximity to market, availability of
utilities such as water, electricity and other infrastructures, ease of access and handling
of human resource, around Abay was selected to locate the plant.

58
6 CONCLUSION AND RECOMMENDATION

6.1 Conclusion
Gypsum was taken from different sources and characterized both physically and chemi-
cally. Physical characterization of the sample shows that:

it is so soft (its hardness is 2.0 Mohs scale) that a fingernail can scratch it and

it is colorless, white, gray, brown, orange, pink, yellow, light red and green.

Chemical characterization of the sample shows that its compositional analysis:

37.4% of CaO, 49.98% of SO3 and 11.03% of H2 O for Kentry gypsum;

38.23% of CaO, 50.43% of SO3 and 11.03% of H2 O for Blue Nile Gorge gypsum;

30.75% of CaO, 44.57% of SO3 and 16.87% of H2 O for Yogef (Lower gypsum bed)
gypsum and

30.99% of CaO, 45.61% of SO3 and 18.67% of H2 O for Yogef (Upper gypsum bed)
gypsum.

All the compositional analysis show that the gypsum quarried from country were best for
chalk production.
In this study, the bulk density and breaking strength in production of quality chalk was
modeled and analyzed through CCD of RSM Design Expert 7.0 version. Particle sizes,
calcinations temperature and moisture content have been employed to carry out the
experimental study. The data was suitably used to explore two factor interactions and
quadratic response surfaces for bulk density and breaking strength respectively and con-
struct second order polynomial models.

The results show that experimental data and data obtained by regression equation closely
correlate each other, which validate the regression equations developed. Therefore, the
present study has shown that RSM combined with a CCD provides a very reliable and ac-
curate methodology for optimizing experiments for the production of quality chalk from
gypsum. Analysis of variance was also found to be significant for both the responses. The
predicted values match with the experimental values reasonably well, with R2 of 0.9991
for bulk density and R2 of 0.9996 for breaking strength.

The Design-Expert software used searches for a combination of factor levels that simul-
taneously satisfy the requirements placed on each of the responses and factors. Opti-
mization requires that goals (i.e., none, maximum, minimum, target, or in range) are set
for the variables and response where all goals were combined into one desirability func-
tion. To find a good set of conditions that meets all the goals, the three variables: particle

59
size (45m - 95m) and moisture content (5% - 7%) were set within range and calcina-
tions temperature (135o C - 145o C) was minimized within range while the responses bulk
density and breaking strength were set in a target.

The mathematical model developed could predict the bulk density and breaking strength
at any point inNPE*100 the experimental domain as well as the determination of the
optimal process parameters. The high correlation in the model indicates that the sec-
ond order polynomial model could be used to optimize the responses. Formulation
with highest desirability (D = 0.998) was selected as optimum. The optimal value ob-
tained 1.1445g/cm3 and 13.85N/cm respectively for bulk density and breaking strength
were found to be 85.55m particle size, 137o C for calcinations temperature and 6.25%
for moisture content as optimum value of process parameters. These results implicate
that the optimization using a RSM based on CCD was useful software in improving the
optimization of quality chalk parameters.

6.2 Recommendation
It is recommended that to use gypsum raw from Derba Mugher site (kentry) as a first
priority.

Because of the quality of gypsum occurrences fulfils the required standard for chalk
and gypsum manufacturing, which was confirmed by chemical analysis.

The supply of raw material from Kentry is adequate enough in the future, as the
resources of Kentry gypsum is in the range of millions of tons.

Relatively lower transportation cost is incurred as compared to the other gypsum

occurrences.

As the supply of the raw materials is in a crushed by the Mugher Cement Enter-
prises, the cost energy to crush at the factory will be proportionally reduced.

There are many factors that affect the quality of chalk but this thesis study considered
only three factors (particle size, calcinations temperature and moisture content), it is
possible to test the other factors such as calcinations time, kerosene to oil ratio of lubri-
cate the moulding and drying time.

This paper also recommends as calcinations kettle can be changed from batch to con-
tinuous and it was used oven dryer for dry a chalk after moulding, it is possible also to
dry by solar without any cost. The obtained quality of chalk was the optimum one, so if
any company was design a factory and work accordingly, by the same selling price with
the existing chalk, it is still feasible.

60
REFERENCES
[1]. Dana E.S., Text Book of Mineralogy. 1945: John Wiley and Sons Inc., New York.
[2] Amene S. and Mojo T., The Geology of Gundo Meskel and Ejere Areas. 1996: Abay
Basin, North Shoa.
[3] Kebede F., Assessment of the Quality of Gypsum in the Northern Highlands of Ethiopia:
2006.
[4] Mamo, H., Limestone and Gypsum Resources at Wolenchite and Femma Area. 1993:
Merhabete, North Shoa.
[5] Dickson T., Gypsum: Mining Journal Metals and Minerals Annual Review. 1998: P. 119.
[6] Branson E.B., Origin of Thick Gypsum and Salt Deposits. Bull.Geo.Soc.Am., 1915: Vol.
26: P. 231-242.
[7] Harben P.W., The industrial minerals handbook, 3rd Edition. 1999: Industrial Miner-
als Information Ltd, London.
[8] Batman A.M., Formation of Mineral Deposits. 1951: John Wiley and Sons Inc., New
York.
[9] Boynton Robert, Chemistry and Technology of Lime and Limestone: 1980.
[10] Adams. G.I., Gypsum Deposits in the United States. 1904: Washington Government
Printing Office.
[11] Carr D., Industrial Minerals and Rocks. Society for Mining, 6th Edition Metallurgy
and Exploration. 1994: Inc. Littleton, Colorado.
[12] Investment Opportunities in Limestone Resources Development of Ethiopia, Geo-
logical Survey of Ethiopia: 2009.
[13] Tesfaye T. and Melka T., Assessment of Cement raw materials in the surrounding.
1993: unpublished report EIGS Mekele, Ethiopia.
[14] Tefera M. and Chernet T., Explanation of the Geological Map of Ethiopia: 1996: Ge-
ological Survey of Ethiopia, Addis Ababa.
[15] Tibebu M. and Hailemichael F., Industrial Minerals and Rock Resource Potential of
Ethiopia. 2003: Geological Survey of Ethiopia, Addis Ababa.
[16] Jelene, Mineral Occurrences Of Ethiopia. 1996: Ministry Of Mine, Addis Ababa.
[17] Mengistu T. and Fentaw H., Industrial Minerals and Rocks Resource Potential of
Ethiopia: 2003.
[18] Sentayehu Zewdie, Opportunities for Gypsum Resource Development in Ethiopia:
2009.
[19] Ulmann A., Encyclopedia of Industrial Chemistry. 1967: Vol. A4: P. 555.
[20] Lorenz W. and Gwosdz W., Manual on the Geological-technical Assessment of Min-
eral Construction Materials. 2003: Germany, Hannover.
[21] Fassil K. and Mitesinot Behailu, Site Characteristics of Adigudom, In Study Report.
1998: Mekele University: Ethiopia.
[22] Dutton J., Global Growth for Gypsum: Lime and Building Products. 1997: P. 2.
[23] Cornelis K. and C.S. Hurlbut Jr., Manual in Mineralogy. 1985: 20th Edition, John Wi-

61
ley Publications: California, USA.
[24] Kreith F. and Bohn M. S., Principles of Heat Transfer. 1997: 5th Edition, PWS Pub-
lishing Company: London.
[25] Jackson Lum, Desk Study on the Red Evaluation of the Potential of the Gypsum De-
posit on Malden Island. 1996: Kiribati.
[26] Coburn A., Gypsum Plaster-Its Manufacture and Use, Intermediate Technology Pub-
lishing: 1989.
[27] Kroschwitz J. I., Kirk-Othmer Encyclopedia of Chemical Technology. 1992: Vol. 6,
Wiley, Chichester.
[28] Ambolt L., The European Plasterboard Industry: Gypsum, Lime and Building Prod-
ucts. 1999: P. 10-13.
[29] Hill H.E., The Transition of Temperature of Gypsum to Anhydrite. Amer.Chem.Soc,
1937: Vol. 59: P. :2242.
[30] Ashmore R., E., Bains & Taylor, The Speed of Calcinations of Mineral Gypsum, BPB
Internal Report. 1961:. 0000321.
[31] Leonard S Roinick, The Stability of Gypsum and Anhydrite in the Geologic Environ-
ment. 1954: Massachusetts Institute of Technology.
[32] Vesna Logar, Production of Calcium Sulphate Alpha-Hemihydrates, in Faculty of
Mining and Geology. 1999: University of Belgrad.
[33] Krueger B., Process for Producing -Hemihydrates Gypsum Crystals From Residue
Containing Dehydrate Gypsum. Ger. 1985: Pat. 3522495A1.
[34] Mcdonald G.J.F., Anhydrite - Gypsum Equilibrium Reactions. American Journal of
Science, 1953: Volume 251: P. 884-898.
[35] Kelvin., Beneficiation of Gypsum and Production of Plaster of Paris. 2003: Federal
University of Technology Minna, Niger State Nigeria.
[36] Acharya. Production of Plaster of Paris Using Solar Energy. 1987: Indian Institute of
Technology Khararpur.
[37] Roinick, L.S., The Stability of Gypsum and Anhydrite in the Geologic Environment.
1954: Massachusetts Institute of Technology.
[38] Wilburn F. W. & Sharp J. H., Journal of Thermal Analysis. 1994: Vol.41: P. 483-492.
[39] Mullick A.K., Gypsum In India: Gypsum. Lime and Building Products, 1999: P. 22-29.
[40] Posnjak E., Deposition of Calcium Sulphate from Sea Water. Am. Journal,Sci., 1940:
Vol. 238: P. 559-568.
[41] Hensen F. E. & Clausen H., Dehydration of Gypsum, In Zem. Kalk. Gips. 1973: Vol.
26(5), P. 223 - 226: German.
[42] Technology Optimization of Wet Flue Gas Desulfurization Process. Chem. Eng.
Technol: Slovenia., 2007: 30(2): p. 220 -233.
[43] Groves W., Gypsum and Anhydrite, in Overseas Geological Surveys,Mineral Resources
Division. 1958: Her Majestys Stationery Office, London.
[44] Mohammad J., Production of Dust Free Chalk from Locally Sourced Gypsum. 2006:
Federal University Of Technology, Minna.

62
[45] Oyelfide, Production of Chalk from Carbide Sludge. 2000: Minna, Niger State.
[46] National Management Consultants PLC. Gypsum Mining, 2006: Processing and Mar-
keting, Government of Pakistan, Islamabad.
[47] Otalora. C.a.F., Formation of Natural Gypsum Mega Crystals in Naica. 2007: Mexico.
p. 327 - 330.
[48] Newland D.H., Geology of Gypsum and Anhydrite. Econ.Geo. 1921: Vol. 16: P. 393-
404.
[49] Worrall W.E., Clay and Ceramic Raw Materials. 5th Edition, 1996, Elsevier Applied
Science Publishers: London.
[50] Zissman., An Introduction to the Rock Forming Minerals. 1992: Pearson Educational
Ltd.: England.
[51] Hancock J. D. & Sharp J., Journal of the American Ceramic Society, 1972: Vol. 55: P.
74-76.
[52] Stone, W.J., and Others Gypsum Deposits in USA. 1920: U.S.Geol.Surv.Bull.
[53] Madeline, Amending soils with Gypsum. 2011: American Society of Agronomy.
[54] Canals and Fermin Otalora., Formation of Natural Gypsum Mega Crystals in Naica.Geology,
2007: Vol. 35(4): Mexico, P. 327 - 330.
[55] Brent Rouppet. Gypsum: Essential for Maximized Water Use Efficiency. 2008: Cali-
fornia.
[56] Kofi Asante, Research Journal of Environmental and Earth Sciences. 2012: Takoradi,
Ghana.
[57] Peter van, Mining water from gypsum, Global Environmental Issues: 2008.
[58] Kelley K.K., Southard J.C., and Anderson C.T., Thermodynamic Properties of Gyp-
sum and its Dehydration Products. U.S.Bull. Mines Tech. 1941: P. 625.
[59] Fraenkel J.R. and N.E.Walen, Design And Evaluate Research In Education,2000: 4th
Edition, Mcgraw-Hill Co. Inc: USA.
[60] Antony, J., Design of experiments for engineers and scientists. 2003: Oxford, Burlin-
ton, MA: Butterworth-Heinemann. p. 152.
[61] Plackett RL, B.J., The design of optimum multi-factorial experiments. 1946: Biometrika:
Londo. p. 305 - 325.
[62] Box P.H., and Hunter J.S., Statistics for Experimenters: An Introduction to Design,
Data Analysis, and Model Building. 1978.
[63] Hamada M., Experiments: Planning, Analysis and Parameter Design Optimization.
2000: New York: Wiley.
[64] M.A. Bezerra, R.E. Santelli, E.P. oliveira and Villar, L.A., Response Surface Methodol-
ogy as a tool for optimization in analytical chemistry. 2008: Talanta, 76, 965-977.
[65] Oktem H, E.T., Kurtaran H., Application of response surface methodology in the opti-
mization of cutting conditions of surface roughness. 2005: Materials Processing Technol.
p. 11-16.
[66] Giovani M., Response Surface Methodology and Product Optimization. 1983.
[67] Douglas C. Montgomery, Design and Analysis of the Experiments. 2001: Arizona

63
State University, New York.
[68] Kansal K, and Kumar P., Parametric optimization of powder mixed electrical dis-
charge machining by response surface methodology. 2005: Materials Processing Tech-
nol., 169(3): 427 - 436.
[69] Mohammed, A., Development of complementary food from maize-cowpea blend,
in Chemical and Bio Engineering. 2012, Addis Ababa University.
[70] Anderson M, White P., RSM simplified-optimizing process using response surface
methods for design of experiments. 2005: Productivity Press, New York.
[71] Singh G. R., Devi V., Optimization of Pellets Containing Solid Dispersion Prepared
by Extrusion/Spheronization Using Central Composite Desigh and Desirability Function
Young Pharm, 2012: Hannover: Germany.: p. 146-56.
[72] Mason.H., Statistical design and analysis of experiments with applications to engi-
neering and science. 2003: J. Wiley: New York. p. 728.
[73] Evans M., Optimization of Manufacturing Processes. 2003: A Response Surface Ap-
proach, Maney Publishing, London.
[74]http://www.Engineering ToolBox.com//
[75]J.W. Eisele, Voluntary Standard Product, National Bereau of Standards,United States,
1971.
[76] Richard W. Felder, Elementary Principles of Chemical Process. 3rd Edition, 2005.
[77] Perry J.H., Chemical Engineers Handbook. 1997: Mcgraw-Hill, New York.
[78] Coulson J.M. and Richardson .J.F., Chemical Engineering. 1997: 3rd Edition, Vol. 6,
Oxford, Pergamon.
[79]. Klaus D. Timmerhau, Plant Design and Economics for Chemical Engineers. 4th Edi-
tion, 1991: Mcgraw-Hill Inc: Colorado.

64
APPENDICES

Table 31: Experimental Design Run Sheet

Parameters Run 1 Run 2 Run 3 Run 4 Run 5
Particle Size (m) 45 70 95 70 70
C
Calcinations Temp (o ) 140 140 135 135 145
Moisture Content (%) 6 6 7 6 7
3
Bulk Density (g/cm ) 1.206 1.150 1.104 1.166 1.125
Breaking Strength (N/cm) 13.2 14.0 12.0 13.8 11.8
Parameters Run 6 Run 7 Run 8 Run 9 Run 10
Particle Size (m) 70 95 70 45 70
C
Calcinations Temp (o ) 145 145 140 145 145
Moisture Content (%) 6 7 7 5 5
Bulk Density (g/cm3 ) 1.135 1.064 1.145 1.193 1.140
Breaking Strength (N/cm) 14.3 12.6 11.5 15.9 16.6
Parameters Run 11 Run 12 Run 13 Run 14 Run 15
Particle Size (m) 95 95 95 70 45
Calcinations Temp (oC ) 135 145 140 140 140145
Moisture Content (%) 5 5 6 5 7
3
Bulk Density (g/cm ) 1.120 1.084 1.093 1.154 1.18
Breaking Strength (N/cm) 17.0 17.5 14.9 16.4 10.8
Parameters Run 16 Run 17 Run 18 Run 19 Run 20
Particle Size (m) 45 95 95 45 45
C
Calcinations Temp (o ) 140 140 145 135 135
Moisture Content (%) 5 7 6 7 5
3
Bulk Density (g/cm ) 1.210 1.088 1.075 1.214 1.225
Breaking Strength (N/cm) 15.7 12.4 15.2 10.2 15.5

Table 32: Design Summary of Designs Expert

Study Type Response Surface
Initial Design Central Composite
Design Model Quadratic Polynomial
Runs 20
Block No Block

65
 Table 33: Regression Coefficient of 2FI and Significance for Bulk Density
Factors Coefficient Estimate 95% CI Low 95% CI High
Intercept 1.15 1.15 1.15
A - PS -0.056 -0.057 -0.054
B - CT -0.017 -0.018 -0.016
3 3
C - MC -7.0010 -8.01410 -5.985103
3 3
AB -1.38510 -2.64010 -1.138104
AC -1.695103 -2.895103 -4.955104

Table 34: Regression Coefficient of quadratic and Significance for Breaking Strength
Factors Coefficient Estimate 95% CI Low 95% CI High
Intercept 14.06 14.02 14.12
A - PS 0.84 0.80 0.87
B - CT 0.26 0.23 0.30
C - MC -2.51 -2.54 -2.47
AC 0.071 0.033 0.11
BC 0.051 0.013 0.089
C2 -0.12 -0.18 -0.063

Figure 25: Perturbation plots for (i) bulk density and (ii) breaking strength

Figure 26: Direct effect of the three factors on the bulk density

66
Figure 27: Direct effect of the three factors on the breaking strength

Figure 28: Effect of two factor interactions on bulk density

Figure 29: Effect of two factor interactions on breaking strength

67
 Figure 30: Contour plots for bulk density

Figure 31: Contour plots for breaking strength

68
Declaration
I, the undersigned, declare that this thesis entitled "Optimization of Gypsum Process-
ing Parameters For the Production of Improved Quality Chalk" has not been submitted
in any form for another degree, diploma or an award at any university or other institution
of the tertiary education. Whenever contributions of others are involved, every effort is
made to indicate this clearly, witH due references to the literature review and discussions.
Iformation taken from the published and unpublished work of the others has been ac-
knowledged in the text and a list of references was give.

The work was under the guidance of Dr. Tassisa Kaba (Asst. Prof.) instructor in Addis
Ababa University, Addis Ababa Institute of Technology, School of Chemical and Bio En-
gineering.

Name

Signature

Place of Submission

Date of Submission
Certification
This thesis has been read and approved as meeting the requirement of the School of
Chemical and Bio Engineering in the Addis Ababa Institute of Technology for the award
of degree of masters of Science in chemical engineering.

Advisor

Signature

Date