ABSTRACT

This industrial training report contains four chapters that explain my 10 weeks
experience in my hosting company, Mineral Research Centre. The content of all chapters
is broadly explained and it is constructed basis on a project assigned. In the opening
chapter, I briefly introduce my hosting company and department for this industrial
training and my schedule during this internship programme. For the second chapter, I
give details about company background including history, mission, vision and the field
work of my department, Advanced Material Technology Section. The third chapter is the
most crucial chapter which explains about a project assigned to me, Preparation of
Synthetic Marble Using Local Mineral of Dolomite and Kaolin. Composite marble or
well known as an artificial marble is a synthetic material which mimic to natural stone
marble. It was made from a mixture of polymer resin and Malaysian mineral filler of
dolomite and kaolin. The main objective of this project is to . The final
chapter of this report explains about the winding up and summary of the project.
 ACKNOWLEDGEMENT

This internship report is an accumulation of many people’s endeavor. But at the

beginning I would like to convey my sincere to the almighty Allah for giving me the
strength and ability to finish the task within the planned time. Then I would like to
express my gratitude to everyone who contributed towards preparing and making this
study successfully. Major contribution was received from the staffs of Mineral Research
Centre (MRC), Ipoh as from Advanced Material Technology Section. To prepare this
internship report considerable thinking and information input from various sources were
involved.

Firstly, I would like to thank to my training officer Mr. Aminudin Mahmud, the
head of Commercialization Section. I would also like to thank to the head of Advanced
Material Technology Section (CTBT), Dr Rashita bt Abd Rashid and research officers,
Pn. Hamizah bt Abdul Samad and Pn. Fauziah bt Muhamad Isa who were also my project
coordinators. The experience and knowledge I gained from them helped me to understand
different elements related to my study.

I would like to express sincere and immense gratitude to my internship supervisor,

Pn. Hamizah bt Abdul Samad, research officer of CTBT in MRC. I am deeply indebted to
her whole hearted supervision to me during the internship period. Her valuable suggestion
and guideline helped me a lot to complete the project assigned and prepare the report in a
well organize manner.

Lastly, I would also like to thank to all the staffs of MRC especially CTBT’s
staffs, Ms Zaidah bt Sulaiman, Ms Nur Shaqirah, Ms. Nurul Syazwani bt Mustaffa, Ms.
Nur Alina Nishaq bt Azman, Mr. Amirul Asyraaf bin Jailani and Mr. Ahmad Azlan bin
Abdullah for helping me while preparing the study by giving suggestion, assistance and
information supply, which were valuable to me. Their helping hand supported me to
complete my task and report successfully.
 CHAPTER 1

1.0 Introduction

Industrial training or internship for sciences student of UPSI (Diploma in Science)

refers to placement of a 2nd year student in an organization to do practical training for 10
weeks. This is one of the most important components of the equipping Sciences graduates
with useful skills in professional content. Trainees are expected to enhance their ability to
manage projects, preparing documentations and deliver presentations.

Students are expected to obtain full time placement at an organization which can
provide appropriate industrial training experience to a future graduate of the Bachelor of
Science. The objectives of internship program are :

 Expose students to working environment

 Expose students to the new technology and knowledge in industry
 Improve knowledge, skills and experience of student with organization
 Increase job opportunity
 To analyze and solve sciences related problems in industry using methods,
tools and techniques learnt in university.
 To demonstrate etiquette and professionalism in science practice.
 To enhances student marketability to be more competitive.

For my industrial training, I was placed at Mineral Research Centre (PPM) at

Jalan Sultan Azlan Shah Ipoh Perak. During the training, I was attached to Advanced
Material Technology Section (CTBT) for 10 weeks. I was assigned to a project entitled
Preparation of Synthetic Marble by Using Local Mineral Dolomite and Kaolin. The
schedule and gantt chart of my industrial training program was attached in the appendix
parts.
1.1 Details of Industrial Training Program

MINERAL RESEARCH CENTRE (MRC)

MINERAL AND GEOSCIENCE DEPARTMENT MALAYSIA (JMG)

ADVANCE MATERIAL TECHNOLOGY SECTION (CTBT)

INDUSTRIAL TRAINING PROGRAMME 2018

1. Programed : Industrial Training Programme 2018

2. Duration : 2 April 2018 – 8 June 2018
3. Section Head : Dr Rashita bt Abd Rashid
4. Coordinator : Pn. Hamizah bt Abdul Samad
5. Supervisor : Pn. Fauziah bt Muhamad Isa (Lead)
Ms. Zaidah bt Sulaiman
Ms. Nur Shaqirah
Ms. Nurul Syazwani bt Mustaffa
Ms. Nur Alina Nishaq bt Azman
Mr. Amirul Asyraaf bin Jailani
Mr. Ahmad Azlan bin Abdullah
6. Student : Ms. Syahira binti Sabri
E20161013295
2nd Year Student
Diploma in Science
Sultan Idris Educational University (UPSI)
7. Title of Project : Preparation of Synthetic Marble Using Local
Mineral of Dolomite and Kaolin.
1.2 Institution Background

1.2.1 Mineral and Geoscience Department Malaysia

Minerals and Geosciences Department Malaysia is a government agency under the

Ministry of Natural Resources and Environment. This department was established on 1st
July 1999 by the merging between Department of Mines and Geological Survey
Department. This merging was a move by the government to restructure the public
agencies along together with global developments and rapid development of the country.
Objectives, core tasks and functions of the two original positions have been processed in
accordance with the current and future needs. As a government agency involved in the
field of mineral and geosciences, the importance of the role is to provide the latest
information and expertise to meet national needs in these areas.

Figure 1.0 : Mineral and Geoscience Department Malaysia Logo

1.2.2 Vision

To make Minerals and Geosciences Department Malaysia as the region’s best

organization in the mineral and geosciences field comparable to the best in the world

1.2.3 Mission

To continue towards enhancing economic competitiveness and quality of life, society and
environment through the effective use of mineral information and geosciences services.
1.2.4 Objectives

Minerals and Geosciences Department Malaysia strives to achieve the following

objectives :

 To provide mineral commodify information to enhance the growth of mineral-

based industries.
 To encourage the optimal use of geosciences information and services for the
sustainable development of country.
 To ensure that mineral resources exploitation expends in a systematic/safe,
efficient and environmentally friendly manner as well as to secure maximum
return to the country.
 To encourage and diversity the use of local mineral resources so as to contribute
towards the development of the country’s industrialization through research and
development (R&D) activities.
 To provides expert services in the fields of the minerals, geosciences and mining
at national and international level so as to promote investment in the mineral
sector and for national development planning.

1.2.5 Functions

 To undertake systematic mineral exploration.

 To undertake systematic investigations in various geosciences disciplines.
 To provide geochemical analyses and physical tests on rock materials and
minerals.
 To acts as the national depository for all information related to geosciences and
mineral resources of the country.
 To collect, analyze and disseminate data and information pertaining to mineral
exploration, mining and related activities.
 To provide technical advisory services and expertise in the fields of minerals,
geosciences, mining and quarrying.
1.2.6 Organization Chart of Minerals and Geosciences Department Malaysia
1.3 Background of Mineral Research Center

Mineral Research Center (MRC) was formerly known as the Mines Research
Institute under the Mines Department Malaysia, Ministry of Primary Industries.

The history of the Mineral Research Centre started way back in 1951 as a small
research division of the Mines Department Malaysia located in Kuala Lumpur. The
establishment of the research division was to revive the production of tin industry which
had experienced a regression during World War II. In view of the many tin mining
activities centered in Perak, the research division was shifted to Ipoh, Perak in 1957. It
was officially opened by the Prime Minister YTM Tunku Abdul Rahman on 4 th May
1957. Mr J.H. Harris became the first Director of the division. In 1973, the status of the
division was elevated to Mines Research Institute.

Since its inception, many investigation works had been carried out in the field of
land evaluation for mining, geotechnical engineering and mineral processing. When the
tin industry collapsed in the mid-1980’s the research of the non-tin minerals such as
ilmenite, monazite, zircon, copper, xenotime, iron, wolframite, bauxite and industrial
mineral like kaolin, marble gravels, silica sand and clay.

Figure 1.1 : Mineral Research Center Ipoh Perak

 On 1st July 1999, the Mines Department Malaysia and the Geological Survey
Department Malaysia merged to become Minerals and Geoscience Department Malaysia.
Under the new Department, the Mines Research Institute changed its name to the Mineral
Research Centre and currently remains as the main government research institute in
minerals in the country. In 2004, a restructuring exercise involving the merger of several
ministries and government departments was carried out to improve the efficiency of the
government machinery. In this exercise the Minerals and Geoscience Department was
placed under the new ministry namely Ministry of Natural Resources and Environments
(NRE) which responsible for the development of the mineral sector.

PPM is committed to sustainable development as well as the optimum utilization

of local mineral resources. As the research wing of the Minerals and Geoscience
Department, MRC undertake mineral R&D activities that are necessary to produce new
technologies and innovations, value-add mineral materials, discover new uses, provide for
safer operation and mitigate adverse environmental impact as well as improve the
competitiveness of the local mineral resources. MRC have made significant achievements
and shall continue to improve along the way. MRC look forwards to establishing as well
as continuing co-operation and co-ordination with other organization both in public and
private sector engaged in mineral research activities and human capital development.

1.3.1 Vision

To become a center of excellence in mineral R&D in the region

1.3.2 Mission

To contribute towards enhancing competitiveness and sustainable development of the

mineral sector through R&D
1.3.3 Objectives

 To encourage and diversity of the use of local mineral resources as to contribute

towards the development of the country’s industrial sector through R&D
 To encourage the development of mineral resources in a sustainable manner
through R&D

1.3.4 Functions

 To carry out R&D on local minerals in order to produce feed and value added
materials for industrial use
 To develop suitable mineral processing and recycling technologies
 To carry out collaborative research with Institute of Higher Learning, other R&D
agencies of industries in the field of mineral
 To commercial significant R&D result through technology transfer to any
interested parties
 To undertake R&D in mineral extraction and its environmental impact as well as
support to the Department and providing services to the industries.
 To assume the role as an advisor and reference center in areas related to search in
local minerals.
 1.3.5 Organization Chart of MRC

There are nine sections available at the Mineral Research Center. Each section has
their own functions in the development of the usage of the minerals in the industries. The
nine sections are :

DIRECTOR OF MINERAL
RESEARCH CENTER

ADVANCED MATERIAL SILICA BASED

TECHNOLOGY SECTION TECHNOLOGY SECTION

CLAY BASED ROCK BASED TECHNOLOGY

TECHNOLOGY SECTION SECTION

MINING AND QUARRYING MINE AND QUARRY

TECHNOLOGY SECTION REHABILITATION
TECHNOLOGY SECTION

MINERAL PROCESSING RESEARCH SUPPORT

TECHNOLOGY SECTION SECTION AND
ADMINISTRATION

ADMINISTRATION AND
FINANCE BRANCH
1.4 Sections in Mineral Research Center

1.4 Advanced Material Technology Section

The idea to study and produce advanced material started way back in 1960’s where
there was a sudden need for ceramics, which have superior or special properties. Research
into producing technical ceramics processing very high tensile or compressive strength,
zero total porosity, infinitesimally low electrical resistant and other outstanding
performance was extensively carried out. Nowadays, people all over the globe are using
at least one product, either consumable or otherwise, made from advanced materials.

In general, advanced material is defined as a new or improved material, which

allows new applications or enhanced in performance through improvements in their
properties, which cannot be achieved before. Advanced materials can be categorized into
advanced metal, advanced ceramics, polymers and composites.

Based on the definition, advanced material will remain advanced as long as there
is continuous need for improvement and advancement in material properties. In this way,
there will be good opportunities for advanced material research to expand planning,
research, production or marketing will be lead the world. A nation with this wealth will
no doubt, has very strong influence on the economy.

1.4.1 Objectives of Advanced Material Technology Section

 To carry out R&D in the purification and synthesis of mineral-based materials,

particularly local minerals, so as transformed into starting materials or precursors
for advanced materials applications, through economic processing technology.
 To become the center for the processing of down-stream mineral product.

1.4.2 Fields of Expertise

 Advanced Ceramic
 Glass Ceramic
 Biomaterials
1.4.3 Projects

Previous Projects :

 Fabrication of thin-film wollastonite

 Synthesis of synthetic diopside using local limestone and silica sand
 Re-utilizing of tin slag and waste glass for producing tile
 Development of biomaterials using local minerals for biomedical and dentistry
application

Current Project :

 Engineered Poly Art Marble

 Dental Leucite Glass Ceramic
1.4.4 Organization Chart

ORGANIZATION CHART

ADVANCED MATERIAL TECHNOLOGY SECTIONS

MINERAL RESEARCH CENTER

Dr. Rashita bt Abd Rashid

Pegawai Penyelidik Q52
Ketua Cawangan

Malek Selamat
Pn Hamizah bt Abd Samad Siti Mazatul Azwa Pegawai Penyelidik Q52
Pegawai Penyelidik Q41 Pegawai Penyelidik Q48

Nur Syaqirah
Zaidah Sulaiman
Pem. Penyelidik Q26
Pn. Fauziah bt Muhd Isa Pem. Penyelidik Q26
Pem. Penyelidik Q22

Nurul Syazwani bt Mustaffa Amirul Asyraf Jailani

Pem. Penyelidik Q19 Pem. Penyelidik Q19

Ahmad Azlan Abdullah

Nur Alina Nishaq Azman Ishak Bakar Pembantu Operasi N11
Pembantu Awam H11 Pembantu Awam H11
 CHAPTER 2

LITERATURE REVIEW

2.1 Introduction of Synthetic Marble

Synthetic marble or cultured marble also known as ‘engineered composite’, is

formed by mixing high strength resin, marble dust and catalyst. Natural marble is
generally heterogeneous with impurities and fractures. They are available in remote areas
and require extensive handling in shaping and finishing. This increase the price for these
stones. To overcome these difficulties, synthetic marble is produced artificially. The
desirable properties in an artificial marble are high mechanical strength, excellent weather
resistance, flexural strength, improved surface hardness, heat resistance, stain resistance,
and an excellent processability.

Cultured marble offers a number of advantages over natural marble. These include
lesser cost and incredible design flexibility compared to stone. They have uniformity in
color and no random variations occurs as in natural stone. Natural marble is limited to flat
surface while cultured marble can easily be formed to one piece bath tub, shower stall etc.
Despite the several advantages offered by artificial marble, it also inherits certain
disadvantages.

For instance, the marble surface can be scratched and care should be taken to
avoid placing objects on it that might cause scratches. Minor scratches or cigarette scorch
marks may be removed by using 600 grit wet or dry sandpaper followed by rubbing and
buffing with standard auto body rubbing compound. However, the safety of marble sinks
can be increased by controlling a number of parameters like deforming time, resin ratio,
hardener amount, oven time, oven temperature and amount of transparent glue
2.2 Chemical Composition

The raw materials required for making cultured marble are filler, resin, gel coat,
solid or liquid pigment and catalyst. Filler acts as an aggregate and must be present up to
85% to 95% by weight. Fillers used can be like aluminium hydroxide, calcium carbonate
and silica. The resin acts like a glue and thereby strengthening the marble. Resin content
in synthetic marble is generally about 12 to 15%. Based on the resin type, artificial
marble can be acrylic or polyester or polycarbonate type. Artificial marbles are prepared
by mixing fillers, pigment and curing agent with a syrup of monomer/polymer, for
examples methyl methacrylate, polymethyl methacrylate, polyester and etc. Thus is
followed by molding the mixture in a mold or a continuous steel belt and curing the
molded mixture.

A study on the complex and multiple

 CHAPTER 3

RAW MATERIALS AND METHODOLOGY

3.1 Raw Materials

The raw materials required for making synthetic marble are filler that consist of
dolomite and kaolin, polyester resin and hardener. The filler acts as an aggregate and
must be present up to 70% by weight. The resin acts like a glue and thereby
strengthening the marble. Resin content in synthetic marble is generally about 12 to 15%.
This part explained the detail of the materials used in the preparation of synthetic marble.

3.1.1 Dolomite

Dolomite is the name of a sedimentary rock and a mineral, both composed of

Calcium Magnesium Carbonate (CaMg(CO3)2) found in crystalline form. In Malaysia,
Dolomite can be found at Perlis and Perak. In this study, the dolomite was collected from
quarry Northern Dolomite Chuping, Perlis (Figure 3.0 ).

The collected sample was dried under the sunlight before undergo sampling
through cone and quartering method. The sample will be analyzed through sample
characterization to obtain information related to the sample. The particle size of dolomite
used in this study is 1.6mm.

Figure 3.0 : Dolomite, ND, Chuping Perlis

3.1.2 Kaolin

Kaolinite is a clay mineral, part of the group of industrial minerals, with the
chemical composition Al2Si2O5(OH)4. Kaolin as found in nature usually contains
varying amounts of other minerals such as muscovite, quartz, feldspar, and anatase.
Kaolin was obtained from Simpang Pulai, Perak. The collected sample was dried under
the sunlight before undergo sampling through cone and quartering method. The sample
will be analyzed through sample characterization to obtain information related to the
sample. The particle size of kaolin used in study is 150ɥm, 75ɥm, 45ɥm.

Figure 3.1 : Kaolin, Simpang Pulai, Perak

3.1.3 Polyester Resin

The type of polymer resin used in this study is polyester resin. Polyester resins are
unsaturated synthetic resins formed by the reaction of dibasic organic acids and
polyhydric alcohols. The resin acts as a binder in the mixture of synthetic marble. In this
study, the amount of polyester resin used is 30% and 25% by weight.

Figure 3.2 : Polyester Resin

3.1.4 Hardener

MEKP is a catalyst used in the composites industry for polyester and vinyl ester
resins. It reacts with the resin to turn it from a liquid to a solid (cure it). MEKP is an
organic peroxide. Since these compounds are unstable in their pure form, they are mixed
with inert compounds to form the catalysts used in the industry. Due to this mixing,
MEKP can be bought in various grades, which can give a range of gel times. Whilst
various types of catalysts are available to cure polyester and vinyl ester resins, MEKP is
the most widely used in contact molding for room temperature cure.

Methyl ethyl ketone peroxide (MEKP) is an organic peroxide, a high explosive

similar to acetone peroxide. MEKP is a colorless, oily liquid whereas acetone peroxide is
a white powder at STP. MEKP is slightly less sensitive to shock and temperature, and
more stable in storage. MEKP was used as hardener with amount of 1% from resin
content (wt%).

Figure 3.3 : Hardener

3.2 Methodology

Raw Materials

Dolomite, Northern Dolomite, Kaolin, Simpang Pulai,

Chuping Perlis Perak

Sampling

Sample Characterization

Characterization of Raw Materials

 Particle Size Analysis (PSA)

 Laser Particle Size Analysis (LPSA)
 Loss On Ignition (LOI)
 Density
 X-Ray Diffraction (XRD)
 X-Ray Fluorescence (XRF)
 Determination of CaO Content
 Determination of MgO Content
3.3 Sample Characterization

Sample :

 Dolomite, Northern Dolomite Chuping, Perlis

 Kaolin, Simpang Pulai, Perak

Before the sample were used in the preparation of synthetic marble, they need to be
analyzed first. There are several tests that need to be carried out on the sample in this
project :

a) Particle Size Analysis (PSA)

b) Laser Particle Size Analysis (LPSA)
c) Loss of Ignition
d) Density
e) X-Ray Diffraction
f) X-Ray Fluorescent
g) Determination of CaO Content (wet method)
h) Determination of MgO Content (wet method)

The purpose of the test and analysis is to find out whether the sample is suitable for the
preparation of synthetic marble. Samples for all tests were prepared by using cone and
quartering method which known as sampling method.
3.3.1 Sampling

Sampling is a small amount of material taken from the main bulk in such a manner that it
is representative of that larger amount. Great responsibility rests on a very small sample,
so it is essential that samples are truly representative of the bulk. To achieve the best
results, the bulk sample should be made as homogenous as possible. If complete
homogeneity of the material is achieved, then every increment obtained by the sampling
method will be representative of the materials. In this activity, the sample used are
dolomite collected from quarry Northern Dolomite Chuping, Perlis and kaolin that was
obtained from Simpang Pulai, Perak. The total sample of dolomite that was collected
from the quarry is 27 bags consist of varieties size of particles, 20-5-mm, <10mm, 1.6mm
and in powder form.

Figure 3.4 : The processing of dolomite at Figure 3.5 : The sample was taken to
quarry Northern Dolomite, Chuping Perlis be processed at MRC

[Link] Cone and Quartering

The sampling by using cone and quartering were dividing small quantities after crushing.
It consist of pouring the material into conical heap and relying on its radial symmetry to
give four identical samples when the heap is flattened and divided by a cross-shaped
metal cutter. Two opposite portion are taken as the samples, whereas the other portions
are being kept as sample reference. The portion that are selected as the sample may again
be coned and quartered, and the processed continued until a sample of the required size is
produced.
Figure 3.4 : Process of cone and quartering method
3.3.2 Particle Size Analysis

Particle size analysis is a procedure used to assess the particle size distribution of
a granular material. In this activity two raw material were involved which is dolomite and
high grade kaolin. For dolomite, the sieve shaker with size 4000mm and below were
used. The total weight of dolomite is 813g. Besides, the sieve shaker with size 2000mm
and below were used for kaolin. The total weight of kaolin is 1.724g.

[Link] Procedure

1. Firtsly, about 1 kg of sample was poured into the sieve shaker.

2. Next, the sieve shaker was closed tightly so that it will not moved when vibrated.
3. The time was set up to 30 minutes to complete the shaker.
4. The process was going on as the sample will pass through from one aperture to
another.
5. After it was completed, the sample was taken outand being weighed.

Figure 3.5 : Sieve Shaker Figure 3.6 : Process of Sieving

3.3.3 Laser Diffraction Particle Size Analysis

The Laser Particle Sizer ANALYSETTE 22 series is a versatile instrument for

determining the size distribution of suspensions, emulsion and powder. It relies on the
fact that diffraction angle is intensively proportional to particle size. As a measuring
principal, laser diffraction boast a few important advantages over the classic methods of
measurement (sieving and gravity sedimention) and over image analysis : fast, accurate
result, no readjustment, wide measuring range and high flexibility. Consequently, it has
now become an established method worldwide and has triumphed over less successful
methods. The instrument is unique in its appearance and impressive in its simplicity while
remaining at the cutting edge of technology.

Mineral Research Center model, the “analysette 22” utilizes a principle of physics,
the scattering of electromagnet waves, to determine particles size distribution. The design
of such instrument is basically quite simple. Particle in parallel laser beam deflect the
light in a fixed, solid angle that depends on the diameter of the particles. A lens focuses
the scattered light in a ring on a sensor that is mounted in the focal plane of the lens;
whereas undiffracted light converges at the focal point on the optical axis. A different
scattering angle is allocated to each individual particle size.

Figure 3.7 : The Laser Particle Figure 3.8 : The sample is inserted
Sizer ANALYSETTE 22 into Analysette 22
3.3.4 Density

The density of a sample was determined using Quantachrome Ultrapycnometer

1000 as shown in figure 3.9. Archimedes concept was applied in this machine where it is
uses nitrogen gas as a medium. Ideally, a gas is used as the displacing fluid since it
penetrates the finest pores assuring maximum accuracy. Helium gas is also recommended
since its small atomic dimension enables entry into crevices and pores approaching two
Angstrom. Its behavior as an ideal gas is also desirable. Two types of samples, dolomite
and kaolin were involve in this analysis. The weight of origin of dolomite is 5.0676g and
kaolin is 3.1782g

[Link] Procedure

1. The sample was put into the container and weighed using weighing balance.
2. Then, the sample was inserted into the pycnometer and closed tightly.
3. The weight of origin of the samples was inserted in the pycnometer.
4. The helium gas has been channeled into the pycnometer.
5. The sample will be run for 40 minutes.
6. The samples was taken out and weighed.

Figure 3.9 : Pycnometer Figure 3.10 : The sample was

inserted into pycnometer
3.3.5 X-Ray Diffraction

X-ray diffraction (XRD) has long been used as a definitive technique for
identifying minerals and other crystalline phases in a wide range of materials. The sample
was made into a fine powder and small portion of the fine powder sample was filled into
the XRD curvette. The curvette with the sample was then loaded into the sample holder of
X-Ray Diffractometer machine (Bruker D8 Advance) equipped with Cu-Kα (λ=1.54Å)
and the sample was then undergoing x-ray diffraction to determine the phase formation
and their evolution of the samples.

The machine has an automated interface with the computer. The sample was
automatically run for 600sec, after which the diffractogram with corresponding data of
intensity versus 2θ are being display on the computer monitor. The diffractogram was
analyzed using Diffracplus BASIC EVALUATION PACKAGE Software database for the
search match of the sample with the database compounds, to obtain the accurate result.

XRD is based on constructive interference where can be obtain when the incident
rays are interacting with the samples due to Bragg’s Law equation :

2d sin θ = nλ

Where d is lattice spacing, θ is diffraction angle, n is order of diffraction peak, and λ is

wavelength of x-ray.

Figure 3.11 : X-Ray Figure 3.12 : The sample was

loaded into the sample holder of
Difractometer Machine
XRD machine
3.3.6 X-Ray Fluorescent

The chemical composition of a sample was determined by X-ray Fluorescent

Spectrometry (XRF) that is capable to analyze a wide range of materials in different
forms for a large part of the periodic table. XRF analyzers determine the chemistry of a
sample by measuring the fluorescent (or secondary) X-ray emitted from a sample when it
is excited by a primary X-ray source. Each of the elements present in a sample produces a
set of characteristic fluorescent X-rays ("a fingerprint") that is unique for that specific
element, which is why XRF spectroscopy is an excellent technology for qualitative and
quantitative analysis of material composition.

[Link] Procedure

1. The sample of dolomite and kaolin are irradiated with high energy X-rays from a
controlled X-ray tube.
2. When an atom in the sample is struck with an X-ray of sufficient energy, an
electron from one of the atom’s inner orbital shells is dislodged.
3. The atom regains stability, filling the vacancy left in the inner orbital shell with an
electron from one of the atom’s higher energy orbital shells.
4. The electron drops to the lower energy state by releasing a fluorescent X-ray. The
energy of this X-ray is equal to the specific difference in energy between two
quantum states of the electron. The measurement of this energy is the basis of
XRF analysis.

Figure 3.13 : X-ray Fluorescent Figure 3.14 : The sample was made into
Spectrometry . button form before loaded into XRF
machine
3.3.7 Loss of ignition

The purpose of this test was to analyzed the loss of ignition of each sample which
are dolomite and kaolin. The loss of ignition usually happened due to the moisture and
impurities (in organic forms) that contained in the sample. The Platinum crucible was
used in this analysis as it has certain characteristic which is a good conductor of heat.

[Link] Procedure

1. Two Platinum crucible were dried in the furnace for each sample of dolomite and
kaolin respectively.
2. Then, the platinum crucibles were taken out and let it cooled in the desiccator for
55 minutes. The cooled platinum crucibles were weighed and recorded.
3. About 1 to 2g of sample was added into the platinum crucibles and was recorded.
4. The furnace was set up at temperature 850˚C and the samples was burned for 1
hour. After that, the sample was taken out and placed into the desiccator for 5
minutes for cooling down.
5. Then, the crucible with burned sample were weighed and recorded. Calculation of
finding the %LOI is shown below :
Loss of sample weight

Initial sample weight X 100

Figure 3.15 : The sample was placed Figure 3.16 : 1. Two Platinum crucible
in the furnace were dried in the furnace
3.3.8 Determination of CaO and MgO contents

The purpose of this test is to determine the percentage contents of CaO and MgO
in both Dolomite from Northern Dolomite, Chuping Perlis by comparing with the
standard Calcium Carbonate. The reagents used in this activity are 0.01M EDTA ,
hydrochloric acid (HCL), 20% Potassium hydroxide (KOH), murexide and eriochrome.
The purpose of using murexide is to determine end point where the color of sample
changed from pink to dark purple. The end point shows CaO was completely neutralized.
While the purpose of eriochrome is to determine end point where the color of sample
changed from purple to blue black. The end point shows MgO was completely
neutralized.

[Link] Procedure

1. To determine the percentage contents of CaO, 3g of standard Calcium Carbonate

and dolomite from Northern Dolomite, Chuping Perlis were dried in the furnace
for 1 to 2 hours at 100˚C. The samples were then let to be cooled in the desiccator.
2. About 0.5g of CaO standard was weighed and poured into the 250ml beaker.
3. Step 2 was repeated for dolomite sample.
4. Then, 100ml of HCL and 100ml of distilled water were mixed together and 20ml
of the mixture was pipetted into the beaker that contains the sample.
5. The samples were then heated up to 125˚C until it dried by using the hot plate as
shown in Figure….
6. After solution was dried, 10ml of HCL was poured into the beaker again to
dissolve the chloride and then it was reheated until the solution completely dried.
7. Next, distilled water was poured into the beaker and brushed it for it to mix well
before being filtered into the 250ml of conical flask.
8. After it has been finished filtered, the distilled water was added until filled up at
the mark point.
CaO

1. Next, 0.01M EDTA was poured into the 100ml pipet. 10ml of CaCO3 had been
pipetted into the 250ml conical flask.
2. 1ml of 20% KOH was then added into the conical flask. Then, a little murexide
was added until the end point where the color of sample changed from pink to
dark purple. The volume of titration was recorded for calculation of percentage of
CaO content. The same procedure was done for standard calcium carbonate.
3. Step 1 and 2 is repeated for the sample of dolomite.

MgO

1. 0.01M EDTA was poured into the 100ml pipet. 10ml of CaCO3 had been pipetted
into the 250ml conical flask.
2. 1ml of buffer was then added into the conical flask. Then, a little eriochrome was
added until the end point where the color of sample changed from pink to dark
purple. The volume of titration was recorded for calculation of percentage of CaO
content. The same procedure was done for standard calcium carbonate.
3. Step 1 and 2 is repeated for the sample of dolomite.
3.4 Preparation of synthetic marble

The molding compositions comprising resin

and filler (dolomite and kaolin) was being
weighed

The mixture of resin and filler have been mixed

by using overheat stirrer for about 5-10 minutes

The molding mixture is poured into a mold

The sample was allowed to cure for 30 minutes

Polishing and grinding of sample

The cutting of sample for analysis purpose

Analysis :

 Compressive Strength
 Flexure Strength
 Barcol Hardness
 Density
 Water Absorption
3.5 Study of Ratio of Dolomite and Kaolin to the Resin

There are 13 formula that have been done and was divided into two part consist of
series 1 and series 2. Series 1 comprising the ratio of dolomite and kaolin to the resin of
30% weight while series 2 with 25% weight of resin. In

Series 1

Filler (wt%)
No. Sample Code Resin (wt%)
Dolomite Kaolin

1 D70 30 70 0

2 D65K5 30 65 5

3 D60K10 30 60 10

4 D55K15 30 55 15

5 D50K20 30 50 20

6 D45K25 30 45 25

Series 2

Filler (wt%)
No. Sample Code Resin (wt%)
Dolomite Kaolin

1 D75 25 75 0

2 D70K5 25 70 5

3 D65K10 25 65 10

4 D60K15 25 60 15

5 D55K20 25 55 20

6 D50K25 25 50 25

7 D45K30 25 45 30

3.6 Analysis
 There are 5 analysis that was conducted on the sample consist of compressive
strength, flexure strength, density, barcol hardness and water absorption. The purpose of
these analysis is to determine the strength and weakness of the sample from variation of
formulas. The diagram below shows the quantities and measurements of the samples
needed for each of the test.

Analysis Measurement, mm No. of sample

Compressive Strength 14mm x 14mm x 14mm 5

Flexure Strength 25mm x 8mm 5

Barcol Hardness 50mm x 50mm x 8mm 1

Water Absorption 14mm x14mm x 14mm 3

Density 14mm x 14mm x 14mm 3

3.6.1 Compressive Strength

 A universal testing machine (UTM), also known as a universal tester, materials
testing machine or materials test frame, is used to test the tensile
strength and compressive strength of materials. The goal of a compression test is to
determine the behavior or response of a material while it experiences a compressive load
by measuring fundamental variables, such as, strain, stress, and deformation. By testing a
material in compression the compressive strength, yield strength, ultimate strength, elastic
limit, and the elastic modulus among other parameters may all be determined. With the
understanding of these different parameters and the values associated with a specific
material it may be determined whether or not the material is suited for specific
applications or if it will fail under the specified stresses.

The measurement of the specimen for this test is 14mm x 14mm. The number of
specimens required for each of sample is five.

[Link] Procedure

1. Dimension of test piece is measured at three different places along its

height/length to determine the average cross-section area.
2. Ends of the specimen should be plane for that the ends are tested on a bearing
plate.
3. The specimen is placed centrally between the two compression plates, such that
the center of moving head is vertically above the center of specimen.
4. Load is applied on the specimen by moving the movable head.
5. The load and corresponding contraction are measured at different intervals. The
load interval may be as 500 kg.
6. Load is applied until the specimen fails.

3.6.2 Flexure Strength

 Flexural testing is used to determine the flex or bending properties of a material.
Flexural testing was done by using Universal Testing Machine (UTM), model of Instron
3367. The UTM which provide many functions and testing was made from United States
of America, USA. Flexural strength test sometimes referred to as a transverse beam test,
as it involves placing a sample between two points or supports and initiating a load using
a third point which are respectively call 3-Point Bend.

When a specimen is placed under flexural loading all three fundamental stresses
are present which is tensile, compressive and shear and so the flexural properties of a
specimen are the result of the combined effect of all three stresses as well as the geometry
of the specimen and the rate the load is applied. Flexural modulus is calculated from the
slope of the stress vs. strain deflection curve. These two values can be used to evaluate
the sample materials ability to withstand flexure or bending forces.

Figure 3.18 : Universal Testing Figure 3.19 : Sample required for

Machine, 3-Point Bend Testing Flexural Strength Test

3.6.3 Barcol Hardness

 Barcol Hardness is used to determine the hardness of both reinforced and non-
reinforced rigid plastics. The specimen is placed under the indentor of the Barcol
hardness tester and a uniform pressure is applied to the specimen until the dial indication
reaches a maximum. The depth of the penetration is converted into absolute Barcol
numbers.

This method is based on the resistance opposed to penetration of a steel needle

pushed by a spring. Results vary on a 0 to 100 scale and provide an estimate of the
crosslink degree of plastic materials and resins both with and without fibers. The number
of specimen needed is one for each of sample. The Barcol Impressor is portable and
therefore suitable for testing the hardness of fabricated parts and individual test specimens
for production control purposes.

Figure 3.21 : Barcol Impressor Figure 3.22 : Pressure is applied to

the specimen

3.6.4 Water Absorption

 Water absorption is used to determine the amount of water absorbed under
specified conditions. Factors affecting water absorption include type of plastic, additives
used, temperature and length of exposure. The data sheds light on the performance of the
materials in water or humid environments. The specimen for the absorption test shall
consist of three representative from each of the samples. The specimen shall have had
their rough edges or loose particles ground off.

[Link] Procedure

1. Three specimens from each samples with dimension 14mm x 14mm were being
weighed using weighing balance.
2. The specimens was then submerged in 250ml conical flask filled with distilled
water for 24 hours.
3. In the next day, the specimens were removed from the water, the surface water
was wiped off with a damp cloth and weighed.
4. The water absorption of each specimen was calculated to the nearest 0.1% as
follows:
Absorption, % = 100(Ws – Wd)/Wd
Where:
Wd = dry weight of the specimen, and
Ws = saturated weight of the specimen after submersion in water.
5. The average water absorption of all specimens is calculated and recorded.

Figure 3.23 : The sample required Figure 3.24 : The sample was
for water absorption test soaked in the distilled water
 CHAPTER 4

RESULTS AND DISCUSSIONS

4.0 Results and discussions are divided into two parts :

i. Characterization of raw minerals of dolomite and kaolin.

ii. Analysis test of sample dolomite and kaolin due to different ratio to the resin.

In this chapter will explain the result of characterization raw mineral using local
dolomite from quarry Northern Dolomite, Chuping Perlis and kaolin from Simpang Pulai,
Perak. The results of analysis test of sample also will be discussed
4.1 Characterization of raw minerals

4.1.1 Particle Size Analysis

Table 4.1 : Particle size distribution of dolomite sample from Chuping, Perlis

Particle Size Weight of Sample Percentage og A subtle set of

(ɥm) (g) Weight of Sample percentages (%)
(%)
10000.00 0.00 0.00 100.00

-10000.00 + 4000 0.00 0.00 100.00

-4000 + 2000 653.00 80.42 19.58

-2000 + 1000 149.00 18.35 1.24

-1000 + 600 0.22 0.03 1.21

-600 + 250 0.39 0.05 1.16

-250 + 150 0.54 0.07 1.09

-150 + 75 1.45 0.18 0.91

-75 + 45 2.20 0.27 0.64

-45.00 5.23 0.64 0.00

Total 812.03 100.00

Total weight of sample : 813.00g

 Particle Size Weight of Sample Percentage og A subtle set of
(ɥm) (g) Weight of Sample percentages (%)
(%)
10000.00 0.00 0.00 100.00
-10000.00 + 4000 0.00 0.00 100.00
-4000 + 2000 600.00 34.93 65.07
-2000 + 1000 176.26 10.26 54.81
-1000 + 600 93.05 5.42 49.39
-600 + 250 193.43 11.26 38.13
-250 + 150 149.83 8.72 29.40
-150 + 75 147.87 8.16 20.79
-75 + 45 211.67 12.32 8.47
-45.00 145.49 8.47 0.00
Total 1717.60 100.00
Table 4.2 : Particle size distribution of kaolin sample from Simpang Pulai, Perak

Total weight of sample : 1724.00g

``````````````````````

Figure 4.1 Particle size distribution of dolomit and kaolin

4.1.2 Laser Diffraction Particle Size Analysis

Sample d50

Dolomite 9.101 ɥm

Kaolin 7.199 ɥm

Table 4.3 :
4.1.3 Density Analysis

The results of density analysis for dolomite, Chuping Perlis and kaolin Simpang
Pulai are shown in the Table 4.4. The average density of dolomite is higher compared to
kaolin. The average value of density is in the range between 2.5260 to 3.0463 gcm-3. The
density value of dolomite is relies under the typical density value of dolomite which is in
the range between 2.8 to 2.9 gcm -3. While, the typical density value of kaolin is 2.65 gcm -
3
.

Sample Density (g/cc)

Dolomite 3.0012

Kaolin 2.8973

Table 4.4 : The average density of dolomite and kaolin

4.1.4 Loss on Ignition Analysis (LOI)

` Table 4.5 shows the results of percentage weight loss for the sample of dolomite
and kaolin when it is strongly heated. The LOI values obtained refers to the carbonate
decomposition, hydrated water, organic substance and others that contained in the sample.
LOI for sample of dolomite and kaolin was done under temperature of 850˚C.

Sample LOI (%)

Dolomite

Kaolin

Figure 4.5 : LOI values for sample of dolomite and kaolin