POLITEKNIK TUN SYED NASIR SYED ISMAIL

THE STUDY OF INFLUENCE OF PALM OIL AND

SUNFLOWER OIL METHYL ESTER BLENDING ON

CLOUD POINT PROPERTIES

NAME MATRIC NO.

PAVITHRA A/P GUNADASS 33DFO17F1015

LIM BOON SIANG 33DFO17F1004

JABATAN TEKNOLOGI KIMIA DAN MAKANAN

JUNE 2019
 ABSTRACT

The objective of this research was to study the influence of blending palm oil
biodiesel and sunflower biodiesel to their cloud point. Cloud point is the point where
the biodiesel started to become cloudy during low temperature that made the biodiesel
to start waxing. It will affect the quality of biodiesel when storage and filtering in cold
condition. Palm oil biodiesel had cloud point of 17.9°C and sunflower biodiesel had
cloud point of 0.1°C. The sample that was studies in this research was a blend of palm
biodiesel and sunflower biodiesel at ratio 10:0, 8:2, 6:4, 5:5, 4:6, 2:8 and 0:10. The
sample was produce from RBD palm oil and sunflower seed oil through trans-
esterification by methanol and a catalyst. Then, the biodiesel is washed with distilled
water to remove other content. 3/27 Intermediate Glyceride Test was used to test the
biodiesel to meet ASTM standard. Blending was undergone using a vortex mixer to
mix well. The ratio for the blend of the palm biodiesel and sunflower biodiesel was
8:2, 6:4, 5:5, 4:6 and 2:8. To test the cloud point, the sample was cooling 1°C by 1°C
until the sample become cloudy. From the observation, the cloud point of blend palm
biodiesel and sunflower biodiesel decrease as the ratio of sunflower biodiesel
increases.

i
 ABSTRAK

Objektif untuk kajian ini adalah untuk mengkaji impak bagi campuran di antara
biodiesel yang diperbuat daripada minyak sawit dan minyak biji bunga matahari
kepada takat keruh. Takat keruh merupakah suhu dimana biodiesel mula berbeku dan
menghasilkan wax. Wax itu mangakibatkan kualiti biodiesel berkurang semasa
simpanan dan penapisan.dalam keadaan yang sejuk. Takat keruh untuk biodiesel
minyak sawit adalah 17.53°C dan biodiesel minyak biji bunga matahari mencapai
0.83°C. Sampel untuk kajian ini merupakah campuran di antara biodiesel minyak
sawit dan biodiesel minyak biji matahari pada nisbah 10:0, 8:2, 6:4, 5:5, dan 0:10.
Sampel tersebut diperbuat daripada RBD minyak sawit olein dan minyak biji bunga
matahari melalui transesterifikasi dengan methanol dan sejenis pemangkin. Kemudian,
air tulen digunakan untuk mencuci biodiesel sampel bagi mengurangkan kemurnian.
3/27 Intermediate Glyceride Test digunakan untuk menguji sampel yang dihasilkan
memastikan ia mengcapai tahap ASTM. Campuran secara fizikal mengunakan vortex
mixer untuk mencampurkan kedua-dua biodiesel.. Untuk mengkaji suhu keruhnya,
suhu sampel dikurangkan sampai keruh diperhatikan. Daripada pemerhatian, suhu
keruh pada nisbah campuran diantara biodiesel minyak sawit dan biodiesel biji bunga
matahari berkurang apabila nisbah biodiesel biji bunga matahari meningkat.

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 STUDENT DECLARATION

I/we hereby declare that this writing to be the result of my/our own research, unless
otherwise noted. I/we also acknowledge that this document had not been presented to
any other diploma or other institutions in particular before or the same time.

PAVITHRA A/P GUNADASS 33DFO17F1015

Signature : Date :

LIM BOON SIANG 33DFO17F1004

Signature : Date :

iii
 LECTURE’S APPROVAL

VERIFICATION OF FINAL PRODUCT

This research study, entitled “ The Study of Influence of Palm Oil and Sunflower Oil
Methyl Ester Blending on Cloud Point Properties”, was prepared and submitted and
also considered satisfactory in terms of scope, reliability and presentation as a partial
compliance with the Chemical Technology Diploma requirement.

……….…………………………….

( Ms. Nor Aziyan Binti Mohd

Nasir )

Supervisor

I confirm that I have reviewed and read this study and in my opinions was that the
nature and performance of the final report for the Diploma of Chemical Technology
was lawful and appropriate in it’s entirely.

…………………………………..

( Pn. Aina Fathiah Binti

Zuihaidi )

Advisor

iv
 ACKNOWLEDGEMENTS

After an intensive period of six months, today will be the day of successfully
done writing this thesis as the finishing of our final year project on our proposal. It has
been such a long period and intense learning for us, not only in the this course but also
in our personal life. Writing this project gives us a great impact. We would like to
reflect on the people who have supported and helped us so much throughout this
whole semester.

First of all, a special thanks to all our DFO lectures for their helpful
collaboration, support and help us to complete this project successfully. We would
particularly send our appreciation and thanks to our supervisor, Ms. Nor Aziyan Binti
Mohd Nasir, thank you for your excellent cooperation and for all the guidance that
were given for our project and further our thesis at Chemical Technology. In addition,
we would also like to thank Madam Aina Fathiah Binti Zuhaidi, for the valuable
teaching and guidance.

We would like to thank our parents also for their wise advices and sympathetic
ear who always there for us. Last but not least, thanks for all my friends and
classmates for sharing their ideas to complete this project.

v
 TABLE OF CONTENT
ABSTRACT I
ABSTRAK II
APPROVAL OF PROJECT III
ACKNOWLEDGE IV
TABLE OF CONTENT V
LIST OF TABLE VII
LIST OF GRAPH VIII
LIST OF FIGURE VIII

Chapter 1
1.1 Introduction 1
1.2 Research Background 2
1.3 Problem statement 3
1.4 Project Objective 4
1.5 Project Scope 4

Chapter 2
2.1 Introduction 5
2.2 Palm oil 6
2.2.1 Palm oil production 6
2.2.1 Palm oil composition 7
2.3 Sunflower oil 8
2.4 Biodiesel 9
2.4.1 Biodiesel production 10
2.5 Chemical analysis 10

Chapter 3
3.1 Introduction 12
3.2 Material and equipment 12
3.3 Preparation of sample 13
3.4 Purification of biodiesel 14
3.5 3/27 Intermediate glyceride test 15
3.6 Blending 16
3.7 Cloud point test 17
3.8 Summarize of chapter 17

Chapter 4
4.1 Introduction 18
4.2 Formulation of biodiesel production 19
4.2.1 Palm oil 19
4.2.2 Sunflower oil 20
4.3 Purification of biodiesel 21
4.3.1 Palm oil 21
4.3.2 Sunflower oil 23
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 4.4 3/27 Intermediate glyceride test 25
4.4.1 Palm oil 25
4.4.2 Sunflower oil 26
4.5 Cloud point test 27
4.6 Summarize of chapter 29

Chapter 5
5.1 Conclusion 30
5.2 Suggestion 32

Appendix

vii
List of Table Pages

Table 3.1 table for data analyze for palm oil and sunflower seed oil 13
biodiesel production for each batch
Table 3.2 table for yield of production for washed biodiesel obtained for 14
each batch
Table 3.3 table for 3/27 intermediate glyceride test for each batch 15
Table 3.4 table for volume of biodiesel needed for each ratio of blending 16
Table 3.5 table for cloud point test for each ratio of blending 17
Table 4.1 table for formulation of palm oil biodiesel production 19
Table 4.2 table for formulation of sunflower seed oil biodiesel production 20
Table4.3 Table of production yield for each batch of palm biodiesel 21
Table 4.4 Table of production yield for washed biodiesel for each batch 23
of sunflower biodiesel.
Table 4.5 table of 3/27 intermediate glyceride test for each batch of 25
washed palm biodiesel
Table 4.6 table of 3/27 intermediate glyceride test for each batch washed 26
sunflower biodiesel
Table 4.7 table of cloud point for each ratio 27

List of Graph Pages

Chart 4.1 charts for production yield of washed biodiesel for each batch 21
of palm oil biodiesel
Chart 4.2 charts for production yield of washed biodiesel for each batch 23
of sunflower seed oil biodiesel
Graf 4.1 graph of cloud point for each ratio 28

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List of figure Pages

Figure 1.1 Small scale palm oil production machine 7

Figure 1.2 fatty acid composition for palm oil 8

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 CHAPTER 1

INTRODUCTION

1.1 INTRODUCTION

From the observation that we have made in this project, in era of technology,
oils are very important sources in our daily life to be used in many ways such as
cooking, dairy products, personal care, surfactant, pharmaceutical, transportation fuel
and many. Oils basically can be divided into two categories which widely known as
edible oil and non edible oil. Edible oil can be in solid (fat) or liquid. Edible oils
defined as a “food substances” or a dairy products of variety origin, sources or
composition that is manufactured for human consumption. Non edible oil strictly not
for human consumption and widely used as diesel or lubricant.

In this project, a green bio diesel fuel was from vegetable oils which is palm
oil and sunflower oil. The palm olein is mainly used for the production of biodiesel.
The biodiesel from palm oil has a good standing for being an alternative and
sustainable fuel in diesel engine. Sunflower oil is the oil which consider has non-
volatile oil pressed directly from the sunflower seeds, thus sunflower oil is one of the
option for biodiesel production at a large scale on its mass cultivation. The reason
why most biodiesel derived from vegetable oil because it is consider to be alternative
and clean fuels for compression ignition engines. Also these vegetable oils are easily
can get in our nearest places, since our Malaysian is the second biggest is the second
biggest country in the world planting palm oil and producing palm oil products. This
will increase the economic balance for our nation and also to stop the accusation of
European side country which giving bad comments towards palm biodiesel.

1
 Biodiesel is one of the biofuel that is sustainable and an alternative fuel for
diesel engine. It can be derived from edible oils by esterification process and which
mostly known as fatty acid methyl ester (FAME). This derivative product (FAME)
has it benefits in low toxicity, high lubricity and high biodegradability compare to
conventional diesel fuel. However, one of the weak point biodiesel produce from
edible oil has higher cloud point. As an alternative way to overcome this problem, we
decided to blend the FAME from palm oil and FAME from sunflower oil in my ratios.
The bleding of two different FAME’s will reduce the cloud point.

In general term, the biodiesel declare as a proper method to reduce the

pollutants emissions from the engine because the oxygen in biodiesel fuel promotes
combustion. Thus, it is important to analyse the relationship between the mixing ratio
of biodiesels and engine emissions. From the result of different mixing ratios, the best
blended biodiesel will be gained according to the country’s temperature.

1.2 RESEARCH BACKGROUND

The depleting of the fossil fuel resources and petroleum reserves in the world,
accelerated the search for an alternative sources for petroleum-based fuel, including
diesel fuels. Throughout a research, it is stated that biodiesel fuel ( fatty acid methyl
ester ) from vegetable oils is considered as the best candidate for diesel fuel substitute
in diesel engines. Since Malaysia is one of the biggest producer of palm oil and palm
oil products, it is a chance to produce palm biodiesel. However the disadvantages are,
any biodiesel derived from palm oil, has the chance of higher cloud point. Cloud point
in any fuels could result in blocking and damages. Studies of the weakness will be
very useful to improve biodiesel production. Therefore, our study is to overcome the
problem by blending two different fatty acid methyl ester in order to reduce cloud
point.
2
1.3 PROBLEM STATEMENT

As the world now chasing towards technology, our nature resources keep
decreasing, thus, the increment of an alternative fuel such as biodiesel is very
important. Based on the observation, a significant rise shows in the usage of biodiesel
from the year 2017 to the current year and data shows that the use of biodiesel will
continue rise due to need of social towards greener product.

On the other hand, a rising problems such as the rising cost of fuel in the
market, global warming and increase in health risk respiratory diseases caused by the
harmful by products of petroleum-based fuels burning. Another problem is increased
amount in the Greenhouse gases at the atmosphere because of the high emission
carbon dioxide, CO2 which will produce from the incomplete combustion of fuel in
engine. Lastly, emission of pollutants such as nitrogen oxide, also released from the
incomplete combustion of fuel in engine.

3
1.4 RESEARCH OBJECTIVE

The objectives of this research are :

i. To synthesize fatty acid methyl ester from palm oil and sunflower by trans
esterfication process.

ii. To reduce the cloud point of palm biodiesel through blending.

iii. To prove the unsaturation of oil will affect the cloud point properties of biodiesel
production.

1.5 SCOPE OF THE RESEARCH

In this study, food grade palm oil with Makmur brand and sunflower oil
produced by Delima Oil product Sdn Bhd are bought from 99 Speedmart Pagoh Jaya
1. Both oil been chosen as the source of fatty acid methyl ester production. All the
chemicals used in this research were reagent grade, for example methanol and
potassium hydroxide (catalyst). These are the chemical used for the trans esterification
process. Also the cloud point analysis of blended biodiesel of different ratios was done
bt water bath method. Lastly, the biodiesel was analysed with glyceride intermediate
test for the ASTM standard biodiesel.

4
1.6 SIGNIFICANCE OF THE PROJECT

In this project, we manage to find a alternative way to overcome the

depletion of fossil fuels resources by producing fatty acid methyl ester which known
as biodiesel from the most founded vegetable oils including palm oil and sunflower
oil. This findings specified more to the cloud point of the blended biodiesels and will
contribute economical support to our country. Since this product are produced from
the trans esterification process, it is not harmful to the environment. Besides that, this
product is totally biodegradable and sustainable for diesel engine. Lastly, it will fully
combustion in the engine, thus, less carbon dioxide will produce.

1.7 RESEARCH HYPOTHESIS

In this study, we concluded an analysis for our product which is fatty acid
methyl ester (biodiesel). We want to produce ASTM standard biodiesel by testing our
product through glyceride intermediate test. Once our biodiesel reaches the ASTM
standard, we proceed blending process of two different biodiesel from palm oil and
sunflower oil. Lastly, we also analyzed the cloud point in the blended biodiesel as our
main result.

5
1.8 SUMMARY OF CHAPTER

Built up on this research, the base of this investigation has been determined
after went through the journals regarding the production of biodiesel and the all the
analysis, the knowledge has been perceived. Moreover, the objectives stated were the
target over this investigation to be achieved. Meanwhile, the researches being in
progress, all the data were recorded in every section of biodiesel production and also
the analysis.

Furthermore, from the journal, we had decided to produce biodiesel using trans
esterification process using condenser soxhlet. In order to achieve the ASTM
standard, intermediate glyceride test been analysed. Testing the cloud point for each
type of biodiesel. Blending two different biodiesel to reduce the cloud point.

Other than that, this research basically gives an alternative solution for the
depleting natural fossil fuels resources. The study of influence of palm biodiesel and
sunflower biodiesel blending on cloud point properties will be explained further in the
literature review.

6
 CHAPTER 2

LITERATURE REVIEW

2.1 INTRODUCTION OF CHAPTER

This chapter covers the studies of fatty acid methyl ester production,
chemical analysis on the FAME produced and the blending properties of two different
fatty acid methyl ester (FAME), also conduct physical study which is to determine the
cloud point of the blended palm biodiesel and sunflower biodiesel.

2.2 PALM OIL

Palm oil is the most widely used vegetable oil. It comes from the fruit of the
African oil palm tree Elaeis guineensis. The oil palm gives highest yields per hectare
of all oil crop present . The fruit of the palm is a central hard-shelled nut surrounded
by an outer pulp (mesocarp) which contains the crude palm oil and the nuts contain
the palm kernel oil ( R.H.V Corley, 2003 ) . Oil palms are originally from Western
Africa, but can flourish wherever heat and rainfall are abundant. Today palm oil is
grow throughout Africa, Asia, North America and South America, with 85% of all
palm oil globally produced and exported from Indonesia and Malaysia ( P.B.
Tinkle, 2003 ).

Malaysia is the second biggest country for the palm oil plantation and in
exporting products derived from palm oil. Malaysian palm oil is goodness because
grows in Malaysian’s sustainable plantations. This palm oil consider to be the non -
GMO oil which is extremely versatile and has been enjoyed by billions for many
years. It is widely used in food and non-food products worldwide.
7
 Palm oil is semi-solid at room temperature and 50 percent saturation level.
Palm oil (and its products) has good resistance to oxidation and heat at prolonged
elevated temperatures hence, making palm oil an ideal ingredient in frying oil blends
(MPOC). Manufacturers and end-users around the world incorporate high percentages
of palm oil in their frying oil blends for both performance and economic reasons.

2.2.1 PALM OIL PRODUCTION

According to Yusof Basiron, 2007, mostly all the palm oil industries in our
Malaysia country are highly organized sectors and the palm oil has a natural head start
in fulfilling sustainability indicators due to its plant physicology of high productivity
and efficient carbon assimilation. Palm oil is derived from the fruit of the oil palm tree
plantation which is grown in tropical regions of Asia and Africa. Then, the fruit
bunches will be harvested and send to the further processes for cleaning and extract
the oil. The final step in palm oil production involves purification of the oil to meet
the demand of various users.

Figure 2.1 Small scale palm oil production machine

Firstly, the palm fruit bunches undergoes sterilization and threshing process.
Sterilization process is done by either roasting or smoking but need a huge amount of
heat in order to soften the fruit bunches and kill the microorganisms. Next, the palm
8
fruit bunches go through threshing process where each piece of fruit is separated from
the bunches. Large palm oil mill plant, will place the palm fruits in rotary drums,
while small palm oil mill will perform threshing process by hand.

After threshing process, this is followed by pressing, where heavy metal

plates are mechanically pressed the fruit to squeeze out the oil. The oil is then diluted
with water and filtered through a screen to help remove debris and impurities. For the
further process, the palm oil refining process. The palm oil refining process can get rid
of the harmful impurities and needless substance in the crude edible oil, getting
standard edible oil by utilizing the physical methods and chemical processes. During
fractionation, palm oil is heated to separates out the various triglycerides contained
within. This helps to separate low-quality oil from higher quality oils, which are rich
in essential fatty acids but contain less saturated fat than unpurified palm oil.

2.2.2 PALM OIL COMPOSITION

Figure 2.2 Palm oil composition

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2.3 SUNFLOWER OIL

Sunflower oil basically is non-volatile oil, pressed from the seeds of the
sunflower. This sunflower oil can be used in many industry such as frying oil,
cosmetics, personal care and also for the production of biodiesel. Basically sunflower
oil is consider to be soft oil and easily can get nearly from all area and shops. This is
due the increment of the sunflower cultivation. Sunflower is a high oil content seed
and average yields can produce 600 pounds of oil per acre, considerably more than
soybeans. There is a great deal of interest from local areas for construction of small
processing facilities such as lab for sunflower biodiesel production. It is recommended
that the sunflower oil be refined and de-waxed before blending it with diesel fuel.

2.4 BIODIESEL

Biodiesel or simply known as fatty acid methyl ester is an alternative fuel for
diesel engine. Fatty acid methyl ester are considered to be environmentally friendly
fuel due to their high biodegradability, low toxicity, low vapor pressure and non
flammable. This biodiesel fuel produce less carbon dioxide, CO2 compare to the
normal gasoline fuel because of the fully combustion of the bodiesel.

Now days, biodiesel gaining more importance as an alternative fuel due to the
depleting of fossil fuels resources . Biodiesel is briefly defined as the monoalkyl
esters of vegetable oils or animal fats. Biodiesel is the best candidate for diesel fuels in
diesel engines. Biodiesel burns like petroleum diesel as it involves regulated
pollutants. On the other hand biodiesel probably has better efficiency than gasoline.
Biodiesel also exhibits great potential for compression-ignition engines. Diesel fuel
can also be replaced by biodiesel made from vegetable oils. Biodiesel is now mainly
being produced from soybean, sunflower, and palm oils.

10
 World energy demand continues to rise. The most feasible way to meet this
growing demand is by using alternative fuels. One such fuel that exhibits great
potential is biofuel, in particular biodiesel (Fernando et al., 2006). The term biofuel
can refer to liquid or gaseous fuels for the transport sector that are predominantly
produced from biomass (Demirbas, 2006). Biofuels include energy security reasons,
environmental concerns, foreign exchange savings, and socioeconomic issues related
to the rural sector (Reijnders, 2006). In developed countries there is a growing trend
toward using modern technologies and efficient bioenergy conversion using a range of
biofuels, which are becoming costwise competitive with fossil fuels (Puhan et al.,
2005).

2.4 .1 BIODIESEL PRODUCTION

Normal lab manual procedure is done for the production of biodiesel for
both palm oil and sunflower oil, which is trans esterification. A number of vegetable
oils can be used to produce biodiesel but for this research we specifically chose palm
oil and sunflower oil. Trans esterification is one of the classic organic reaction that
have applied in numerous laboratory uses and industrial application and on some
occasions, trans esterification is more advantageous than the ester synthesis from
carboxylic acids and alcohols.

According to Junzo Otera, 1993, transesterification is the general term used

to describe the important class of organic reactions where an ester is transformed into
another through interchange of the alkoxy moiety. When the original ester is reacted
with an alcohol, the transesterification process is called alcoholysis.

Trans esterification : simple alcohols are used and this process is usually
carried out with a basic catalyst ( NaOH,KOH ) in the complete absence of water. The
bonding of alcohol and organic acid produces ester. An excess alcohol is needed to

11
accelerate the reaction, with methyl alcohol glycerol separation occurs readily. If
water is present soap is the by-product, which results in decreasing yield of ester. In
the trans esterification process alcohol combines with triglyceride molecule from acid
to form glycerol and ester.The glycerol is then removed by density separation. Trans
esterification decreases the viscosity of the oil, making it similar to diesel fuel in
characteristics.

2.5 CHEMICAL ANALYSIS

For the chemical test, the chemicals used on the fatty acid methyl ester
FAME, are analytical grade. Glyceride intermediate test basically to prove that the
biodiesel produced has achieved the ASTM standard. To determine the biodiesel was
high or low in di-glyceride or mono-glyceride, this test is conducted. According to
Jan Warn Quist, for this chemical analysis, methanol as the solvent to dissolve the
commercial biodiesel in ratio 3ml of the biodiesel sample mixed with 27ml of
methanol in a test tube or small bottle.

. This test is undergoes by a principle which the triglyceride was unable to

dissolve in methanol and di-glyceride and mono-glyceride will result as a cloudy
mixture or emulsion of triglyceride and methanol. However biodiesel can be fully
dissolve in methanol in a clear liquid. The insoluble content which is triglyceride will
remain as a layer at the bottom after settled. To the biodiesel that meet the standard, it
should be remain clear after dissolve in methanol.

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2.6 BLENDING

Biodiesel can be blend with a few solute which soluble in oil through physical
mixing. The palm biodiesel content high in saturated fatty acid which is problem to
the engine because it will cause blockage due to its high cloud point, thus, through
blending process with sunflower biodiesel could reduce the cloud point properties
( industrial crops and products, May 2013 ). After the biodiesel achieved the ASTM
standard, blend both biodiesel through simple mixing process using pipette. All the
blending are follow different ratios, and shake vigorously using the vortex machine.

2.7 PHYSICAL ANALYSIS

For the physical test, cloud point test were analyzed on the fatty acid methyl
ester. Cloud point test is an important test to identify cloud point of biodiesel. It can be
used to estimate the cold filter plugging point which is an important measure in
predict the situation when biodiesel used in cool condition. Biodiesel mostly have
high cloud point than their oil sources. This statement is prove by 2 research from
Frank D. Gunstone “Vegetable Oils in Food Technology Composition, Properties and
Uses Second Edition” and Teoh C. ming” . Strategies for decreasing the pour point
and cloud point of palm oil product.

Based on the research showed above, cloud point of palm olein was located at
2°C-11.5°C, but after methanolysis or trans-esterification of palm olein, the cloud
point increase to 13.5°C. The increasing of at least about 2°C of cloud point becomes
a problem when using in cool condition. Cloud point is the temperature of the fuel
which small solid crystal can be observed as the fuel cools. It is an alternative way or
cheaper way to conducted cold filter plugging point. Cold filter plugging point is the
temperature at which a fuel filter plugs due to fuel component that have crystalized or
sparingly solidified. This could make the blocking of filter when fuel use in cool
13
condition. As a result, the fuel can’t function at the temperature and may damage the
diesel engine. Cold filter plugging point test was expensive and tedious. Therefore,
cloud point is conducted to bracket the temperature at which the fuel will start to fail.

2.8 SUMMARY OF THE CHAPTER

This chapter basically guideline or information from the journals related to our
research title. The information provided about the suitability of the types of oils for
biodiesel production and also the how to produce biodiesel in a manual way. The
sources for this research mainly from the journals, all the journals are related to the
research title. In this chapter the author names and year are been included together
with the point from their journals More clear steps will be explained in the following
chapter which is methodology.

14
 CHAPTER 3

METHODOLOGY

3.1 Introduction

This research is conducted to prove blending between palm oil biodiesel and
sunflower biodiesel would influence their cloud point. As main sample, biodiesel from
palm oil and sunflower oil was produced through chemical reaction. Blending is to
change the cloud point of biodiesel; cloud point of palm oil biodiesel is lowered by
blending with sunflower biodiesel. To get a fully relationship between the blended
biodiesel, different ratio of blending is tested.

3.2 Material and equipment

Food grade palm olein cap Makmur purchased from 99 Speedmart at Pagoh
jaya and their fatty acids were chosen for fatty acid methyl ester production. Adela
food grade sunflower seed oil purchased from Aeon Big at Ampang was chosen as
sources of sunflower biodiesel production. Methanol, sodium hydroxide, distilled
water were all reagent grade. Vortex machine, soxhlet, hot plate and separating funnel
were all provided by Politeknik Tun Syed Nasir.

15
3.3 Preparation of sample

First, volume of oil sample and methanol used is measured by using measuring
cylinder which is 100ml of oil for 20 ml of methanol. Potassium hydroxide is
weighted by using digital weight balance. Then, potassium hydroxide is full dissolve
in methanol, stir the solution until clear liquid is get. After that, soxhlet is setting up to
prepared as reactor for methanolysis of oil. Mix the methanol solution and oil in
soxhlet reactor. Boiling flask is heated up in water bath to 60°C. Stir and heat
continuously the mixture for 2 hour. Finally, after 2 hour mixture is settling down in
closed container for a day.

Type of Volume Volume of Weight of Volume of Volume of

oil/batch of oil(ml) methanol(ml) potassium glycerol(ml) crude
hydroxide(g) biodiesel(ml)
1st batch 200 40 1.8
2nd batch 100 20 0.9
Table 3.1 table for data analyze for palm oil and sunflower seed oil biodiesel
production for each batch

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3.4 Purification of biodiesel

After a day in settling the biodiesel sample, the sample was performed in 2
layers. A lighter upper layer and a darker bottom layer, vortex can be done to observe
the different viscosity or flow rate between 2 layers. Then, the biodiesel with glycerin
is inserted to separating funnel. The 2 layers were separate by a stopper and glycerin
layers were collected by measuring cylinder. The amount of glycerin is measured and
recorded. Then, prepare 50ml of distilled water. Distilled water was inserted into the
separating funnel to wash away glycerin that dissolve in biodiesel. Closed the lid and
shake the sample to mix the biodiesel and water. After that, separating funnel was
placed for settling down the water and biodiesel. Then, separate the water from
biodiesel. Measure the volume of water that discharge after washing. Repeat the step
until the volume of discharge water maintain at 50ml. lastly, the biodiesel was dried in
oven at 80°C for 2hour using beaker. Record the volume of washed biodiesel to get
the percentage of production.

Type of Volume for oil Volume of washed Yield of production

oil/Batch feedstock(ml) biodiesel(ml) for washed biodiesel
(%)
st
1 batch
2nd batch
Table 3.2 table for yield of production for washed biodiesel obtained for each batch

Calculation for the yield of production for washed biodiesel obtained::

Volume of washed biodiesel( ml)

yield of production for washed biodiesel obtained (%)= ×100
Volume of oil feedstock (ml)

3.5 3/27 Intermediate Glyceride Test

17
 Firstly, prepare 27ml of methanol in a test tube. Then, 3 ml of biodiesel sample
was pipetted into the test tube. Current solubility of biodiesel sample can be observed
through the present of oil droplet that fall to the bottom of methanol and become a
layer. Then, test tube was sealed by using parafilm. The mixture was shaking
vigorously for a minute. After that, test tube was placed in test tube rack. The present
of insoluble content and the cloudiness of methanol were observed and recorded.

Type of Cloudiness of Insoluble content Cloudiness of Insoluble

oil/Batch solution in solution solution after content in
shaking solution after
5 minutes
1st Batch
2nd Batch
Table 3.3 table for 3/27 intermediate glyceride test for each batch

18
3.6 Blending

This step was undergoes after the biodiesel passed the intermediate glyceride
test. The blending was mix inside the sampling bottle with the support from vortex
machine. At the initial step, the sampling bottle was dried by using oven in 80°C for
1hours to ensure no moisture content in the bottle. The bottle was labeled according to
the ratio showed on table. Then, palm biodiesel was pipetted into the sampling bottle
according to the volume that showed on table. After that, sunflower also pipetted into
the sampling bottle follow the table above. After the sample was mixed, the sampling
bottle was sealed and vortex using vortex machine for 5 minutes to mix well.

Ratio(palm biodiesel : sunflower Volume of palm Volume of

biodiesel) biodiesel(ml) sunflower
biodiesel(ml)
10:0 20 0
8:2 16 4
6:4 12 8
5:5 10 10
4:6 8 12
2:8 4 16
0:10 0 20
Total used for blending 50 50
Table 3.4 table for volume of biodiesel needed for each ratio of blending

19
3.7 Cloud point test

After the blending was prepared, the final test can be tested on the sample
prepared. The test tube was dried in the oven at 80°Cfor 1 hours. After that, 3ml
of biodiesel sample was pipetted into the dry test tube. Then, the test tube was
cooled in ice bath. The cooling step must be reduce the temperature 1°C by 1°C.
It is because the biodiesel was high sensitive to the cool temperature. Record the
temperature when cloudy was observed at the test tube.

Ratio of 1st cloud 2nd 3rd Average

blending(palm point cloud Cloud cloud
biodiesel : test(°C) point point point(°C)
sunflower test(°C) test(°C)
biodiesel)
10:0
8:2
6:4
5:5
4:6
2:8
0:10
Table 3.5 table for cloud point test for each ratio of blending

3.8 Summarize of chapter

In this chapter, the methods for research are discussed to reach the
objective of target. The biodiesel was produced through trans-esterification.
Finally, the blended biodiesel and their cloud point was analyze to obtain the
effect of blending toward their cloud point.

CHAPTER 4
20
 DISCUSSION

4.1 Introduction

After preparation of biodiesel and biodiesel blend, the objective of this

research was to study the cloud point of biodiesel and blended biodiesel to prove
that cloud point of palm oil biodiesel can be reduce through the physical blending
of 2 type of biodiesel. The result of this research was separately determined by
the formulation for palm oil and sunflower oil, yield of production, intermediate
test and cloud point. The data was analysis through the table that given in
chapter 3. Graf and chart was used to analyze the data that obtain through the
method. In this chapter, those results were discussed and analyze to prove the
objective of this research had achieved. Formulation for each batch palm oil
biodiesel and sunflower biodiesel production can be used for comparing to their
yield of washed biodiesel produced to obtain the highest yield of production.
3/27 Intermediate glyceride was also related to the formulation of each batch.
Cloud point was discussed for each ratio of blending

21
4.2 Formulation for Biodiesel production

The production of biodiesel was undergoes in the type of using batch

reaction. The amount of material use for biodiesel production was constant and
some was manipulated. The crude glycerol and crude biodiesel was obtained
after settling down the separate layers. The result was obtained from the
measuring of crude biodiesel.

4.3.1 Palm oil

Batch Volume of Volume of Weight of Time of Volume of

oil(ml) methanol(ml) potassium reaction crude
hydroxide(g) (hours) glycerol(ml)
1st batch 100 20 0.98 3 15ml
2nd batch 100 20 0.131 2 15ml
3rd batch 100 20 0.98 2 13ml
Table 4.1 table for formulation of palm oil biodiesel production

The table 4.1 shows the formulation for 3 batch of reaction. All the reaction
was conducted in a temperature of 70-80°C. In the table, the crude glycerol that
obtained from 1st batch and 2nd batch was same volume however the 3 rd batch has
less crude glycerol produce. This is because the different time and weight of
potassium hydroxide causes the reaction to be faster or slower. Weight of
potassium hydroxide could affect the reaction, but there is another factor that
more impact to the production of crude glycerol which is time. In the table, the
weight of sodium hydroxide for 1st batch and 3rd batch was same but the time of
reaction was different which the 1st batch of biodiesel production taken 3hours
and the 3rd batch of biodiesel production taken 2 hours for reaction. The higher
the time was taken for biodiesel production, the more crude glycerin was

22
produced by the reaction. However, the weight of potassium hydroxide effect to
the volume of glycerol produces for 1st batch and 2nd batch wasn’t showed
because the amounts of crude glycerol that produce from the reaction are same.
The average for crude glycerin produced for palm oil was14.33ml.The impact of
the different weight of potassium hydroxide wasn’t showed in the biodiesel
production but it will affect the quality of biodiesel that discussed later.

4.3.2 Sunflower oil

Batch Volume of Volume of Weight of Time of Volume of

oil(ml) methanol(ml) potassium reaction glycerol(ml)
hydroxide(g) (hours)
1st batch 200 40 9.3 3 34ml
nd
2 batch 100 20 0.15 2 10ml
Table 4.2 table for formulation of sunflower seed oil biodiesel production

The table 4.2 showed the result for sunflower oil biodiesel production. In the
result, sunflower oil production was produce with different range of factors. Firstly,
the volume of oil and methanol for the 2 batch was different. However the ratio of oil
and methanol still maintain at the same ratio. The volume for oil and methanol that
prepared for 1st batch was doubled for the 2nd batch. The weight or concentration for
potassium hydroxide for the 2 batch is also different which the 1 st batch is taken 9.3g
of potassium hydroxide or 232.5M for concentration when dissolve in methanol and
0.15g of potassium hydroxide or 7.5M for concentration when dissolve in methanol
for 2nd batch. There are 9.15g or 225M different between the 2 batches. The time taken
for reaction also different which the 1 st batch takes 3 hours and the 2 nd batch takes 2
hours for reaction. They resulted the volume of crude glycerol was different which the
volume of crude glycerol that produce for 1st batch is higher was higher than 2nd batch.
The amount of crude glycerol that produce by 1 st batch is higher because the volume
of oil and methanol, concentration of potassium hydroxide and the time taken for

23
reaction was higher than the 2nd batch. This show the increase of volume of oil and
methanol, concentration of potassium hydroxide and the time could increase the crude
glycerol that produced.

4.4 Purification of biodiesel

The crude biodiesel that produce from the trans-esterification cannot be direct use
because there are high amount of soap and glycerin or impurities. To remove the
impurities, washing is used to reduce the soap content. The washed biodiesel will have
lighter colour and clear than crude biodiesel.

4.3.1 Palm oil

Batch Volume for oil Volume of washed Production yield for

feedstock(ml) biodiesel(ml) washed biodiesel (%)
st
1 batch 100 65 65
2nd batch 100 75 75
rd
3 batch 100 92 92
Table4.3 Table of production yield for each batch of palm oil biodiesel

24
 Production yield of washed biodiesel for each batch
100
90
80
70
60
50
40
30
20
10
0
1st Batch 2nd batch 3rd batch

Chart 4.1 charts for production yield of washed biodiesel for each batch of palm oil
biodiesel

From the data that showed the volume for oil feedstock and washed biodiesel
and production yield of washed biodiesel for each batch. 3rd batch have the highest
production yield however 1st batch have the lowest production yield. 1st batch have the
lowest production probably because the spillage of biodiesel when inserted into the
separating funnel. This is human error that causes the reduction of production yield for
1st batch. Other than that, the formulation also will affect the production yield of the
batch. The 3rd batch with high weight of potassium hydroxide resulted higher yield
production than the second batch. Thus, the higher the weight of potassium hydroxide
was used in sample preparation, the higher the yield of production for the batch.
Washing was use to remove the crude glycerin and soap from the biodiesel sample.
Hence the lower the production yield can mean to there are soap and glycerin was
produce during the production or trans-esterification of oil. From the bar chart, 1 st
batch have been the lowest value, which show the more potassium hydroxide and
time, the more soap and glycerin produce.

25
 4.3.2 Sunflower oil

Batch Volume for oil Volume of washed Production yield for

feedstock(ml) biodiesel(ml) washed biodiesel (%)
st
1 batch 200 163 81.5
2nd batch 100 60 60
Table 4.4 Table of production yield for washed biodiesel for each batch of sunflower
biodiesel.

Production yield of washed biodiesel for each batch

90

80

70

60

50

40

30

20

10

0
1st batch 2nd batch

Chart 4.2 charts for production yield of washed biodiesel for each batch of sunflower
seed oil biodiesel

From the bar chart that showed on above, production yield for 1 st batch was
dramatically higher than the 2nd batch. The different between 1st batch and 2nd batch
was approximately reached near to 20%. This shows that the 2nd batch has more
glycerin and soap than the 1st batch. 1st batch has more volume of oil and methanol
compare to 2nd batch in biodiesel production. Hence, the more the volume of oil and
methanol use to produce biodiesel, the less soap and glycerin produce during biodiesel

26
trans-esterification. Because of that, most of the biodiesel industry was using large
scale production to minimize the soap and glycerin produce during trans-
esterification. The statement that the more potassium hydroxide uses in production,
the more sodium hydroxide use in biodiesel production, the higher the production
yield was also proved in this result. The time use to produce biodiesel also
significantly affected the result of the sunflower biodiesel production. Hence, the
production of sunflower biodiesel was very near to the result that get from palm
biodiesel production which the more potassium hydroxide use in palm oil production
the higher the production yield of washed palm biodiesel.

27
 4.5 3/27 Intermediate glyceride test

Washing with distilled water only can remove the compound that soluble in
water. However, there are compound that was insoluble can’t be remove easily. This
test is to indicate those compounds that cannot dissolve in water. The impurities
compound can be separate using fractionation distillation but it need a large amount of
costs. As result, the failed sample will be save or as waste. More batches will be done
until passed this test.

4.4.1 Palm oil

Batch/ Cloudiness of Insoluble content Cloudiness of Insoluble

type of oil solution in solution solution after content in
shaking solution after
5 minutes
st
Palm 1 Clear Not presented Clear Not presented
Batch
Palm 2nd Clear Present Cloudy Present
Batch
Palm 3rd Clear Not presented Clear Not presented
Batch
Table 4.5 table of 3/27 intermediate glyceride test for each batch of washed palm
biodiesel

The table 4.5 shows the test result for 3 batch of palm biodiesel, if the
biodiesel meet the standard which has least amount of impurities, it should be remain
clear in methanol. The1st batch and 3rd batch meet the standard of biodiesel which
solution should be remain clear in the methanol. 2 nd batch does not meet the standard
because an insoluble content observed in the solution. Shaking was use to ensure that
the biodiesel can fully dissolve in methanol. Some compound that sparingly soluble in
methanol will be directed observed after shaking. It indicates as a cloudy solution after

28
shaking. As result from the test, the concentration of potassium hydroxide has affected
on the intermediate glyceride test result. The 1st batch and 3rd batch with 49M is
passed however the 2nd batch with 6.8M could not pass the test. This shows that the
concentrations of potassium hydroxide solution have effect on the impurities that
could not soluble in methanol. However, there are problem when discussed the result
between the intermediate glyceride test and yield of biodiesel production. In the yield
of biodiesel production for palm oil batch 2 and 3, It failed the intermediate glyceride
test. This shows that the intermediate glyceride only showed the presence of glyceride
content in biodiesel and can’t identify the presence of biodiesel in the sample. Because
of that the production of biodiesel is undefined. The addition analysis is needed to
prove the product of trans-esterification was biodiesel. There are also possibilities of
fatty acid that produce during the trans-esterification of oil which made the compound
can’t be defined. If compound analyzing using chromatography was done before this
step the biodiesel can be confirm to be produced.

4.4.2 Sunflower oil

Type of Cloudiness of Insoluble content Cloudiness of Insoluble

oil/Batch solution in solution solution after content in
shaking solution after
5 minutes
1st Batch Clear Not presented Clear Not presented
2nd Batch Clear Presented Cloudy Present
Table 4.6 table of 3/27 intermediate glyceride test for each batch washed sunflower
biodiesel

The table 4.6 shows the result of intermediate glyceride test for each batch of
sunflower oil. 1st batch have been was passed the intermediate glyceride test and 2 nd
batch does not passed the intermediate glyceride test. The significant differences
between the 2 batches was their formulation that mainly cause the result of the pass or
29
fail… 1st batch biodiesel was using high amount of oil, methanol, weight of potassium
hydroxide and time taken for reaction. In test for palm oil, the time taken doesn’t
affect the impurities of biodiesel. As a conclude from the 2 result from the production
of biodiesel for palm oil and sunflower oil the concentration of sodium hydroxide
should be in a range of 49M and 232.5M. For the sunflower biodiesel production also
showed same problem with the palm oil biodiesel production which is the product
can’t be identified as biodiesel and their characteristic only solubility in methanol was
tested. The information that obtained doesn’t enough to identify the biodiesel
compound in the sample.

30
4.5 Cloud point test

After the main sample which is the blended biodiesel was prepared, the final step
which is to determine the cloud point for each sample can be done. The requirement
for the sample that can be use was passed through the intermediate glyceride test
which indicates the impurities in biodiesel. The impurities in biodiesel may affect the
cloud point of the biodiesel. Thus, the preparation of biodiesel should be carefully.

Ratio of Cloud point Cloud point Cloud point Cloud point

blending First test(°C) Second Third test(°C) Average(°C)
(sunflower test(°C)
: palm)
10:0 0.8 -0.2 -0.3 0.1
8:2 4.7 5.7 4.8 5.07
4:6 5.4 6.3 6.3 6.00
5:5 10.8 9.8 10.4 10.33
6:4 12.7 11.6 11.1 11.8
2:8 13.2 12.5 12.4 12.7
0:10 18.2 18.1 17.4 17.9
Table 4.7 table of cloud point for each ratio

31
 Ratio of blending affect cloud point
20
18
16 f(x) = − 2.66 x + 19.76
R² = 0.96
Cloud point average

14
12 Ratio of blending cloud point
10 Linear (Ratio of blending cloud
point)
8
6
4
2
0
0 2 4 5 6 8 10
Ratio of blending for sunflower biodiesel

Graf 4.1 graph of cloud point for each ratio

The graph shows the relation between the ratio of blending and their cloud point.
R² is a measure the strength of the relationship of the relationship between the
variable. The strongest relationship was 1. The value that between 0.99 and 1 show
that there are significant relationship between the 2 variable. The value of R² for the
line above was 0.9613 which is in the range between 0.99 and 1 show that there are
significant relationship between the cloud point and ratio of blending. The cloud point
for the palm biodiesel was 17.9°C. There is doubt that palm biodiesel may freeze at
17°C. Palm oil which is a hard oil as expected have high cloud point in biodiesel
which is 17.9 and sunflower oil which is a soft oil also as expected which has low
cloud point which to 0°C. As summarize, the saturation of oil as sources for biodiesel
production will affect the cloud point of the biodiesel that produced. The cloud point
for biodiesel was decrease as the ratio of sunflower biodiesel decrease. This proves
that the cloud point of the biodiesel will change due to the blending of different oil.
Sunflower biodiesel can decrease the cloud point of palm biodiesel until 5°C which it
can use in a few countries that have no snow but with low temperature. Because of the
biodiesel can’t be identified, the cloud point test for biodiesel became inaccurate.

32
There are unidentified compound that may affect to the cloud point of biodiesel. A
research shows that glycerin could lower the cloud point. There were also other
compound such as monoglyceride, diglyceride, moisture content and dirt. have effect
to biodiesel cloud point was researched by Anup Pradhan, student from University of
Idaho.

4.6 Summarize of chapter

In this chapter, the result of formulation, production yield of washed biodiesel and
cloud point for each ratio of blending was successfully obtain from the method and
presented through table, graph and chart. The data are discussed to obtain the highest
production yield of biodiesel and the cloud point of blended biodiesel for different
ratio.

33
 CHAPTER 5

CONCLUSION AND SUGGSTION

5.1 INTRODUCTION

As the result, all the objectives of this research have been successfully
achieved and this research complete on the time. Based on the knowledge from the
literature review, it can be seen that there are many ways to produce palm biodiesel
and methods to analyse the biodiesel. This research proves commercial biodiesel can
be produced through trans esterification process. Also from the journal, a ASTM
standard biodiesel was produced by intermediate glyceride test. Though the cloud
point test, it can determined the waxing properties of the biodiesel.

5.2 CONCLUSION

As a conclusion, biodiesel is the most needed innovation which will be used

in future and has it own benefits. This biodiesel will be an alternative fuel for the
fossil fuels. In future also, vehicle industries will focus on producing more diesel
engine cars and more vehicles.

In this study, both chemical test and physical test were conducted on our
biodiesel in order to achieve our objectives. Therefore, in this analysis, a ASTM
standard biodiesel produced through glyceride intermediate test. The different

34
biodiesel are blended successful in many ratios and as for our main test which is cloud
point test is conducted on blended biodiesel and gives a good result.

Based on the objectives that had been done, to synthesize the fatty acid
methyl ester, FAME from palm oil and sunflower oil was successfully produced
through trans esterification process. This biodiesel is been proven by the glyceride
intermediate test. From the test, it shows that the produced biodiesel achieved the
ASTM standard.

For the next objective, to reduce the cloud point of palm biodiesel through
blending with sunflower biodiesel. About 7 blended samples was prepared according
to the ratio by using simple mixing process. Referring to the results received, For our
country the ratio palm biodiesel 2:8 sunflower biodiesel is good. Maybe for the other
ratios which shows lower cloud point can be exported to other country.

Finally, for the last objective to prove the unsaturation of oil will affect the
cloud point properties in biodiesel production. Palm oil role as the hard oil whereas
the sunflower oil as the soft oil. This differences in unsaturation brings an equality in
the end product which is biodiesel. Hard oil means solidify faster compare to the soft
oil which solidify slowly.

The conclusion of the whole research, biodiesel is an alternative fuel and

contributes to green technology since it is sustainable and biodegradable. This
biodiesel is a derivative product from vegetable oil and will be used as commercial
biodiesel in future for all types of diesel engines.

35
5.3 SUGGESTION

In future, with all the suggestion given to us, we will produce biodiesel from
many types oils with a great quality, maybe low cost but great quality oil will be used
such as jatropha oil, soybean oil or corn oil. More equipment and instrument will be
used to identify each compounds present in the biodiesel, for an example gas
chromatography, this instrument will analyse the compounds presence in the
biodiesel in more details. We will increase some analysis for testing the biodiesel such
as flash point, viscosity, smoke point and combustion properties. Both chemical and
physical analysis will be conducted on the biodiesel to improve the efficiency of the
diesel fuel. A more purified biodiesel will be produced in future through the ASTM
standard.

36
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39
APPENDIX Diagram 1.3 product after palm oil
trans-esterification

Picture for palm and sunflower oil

preparation

Purification of biodiesel sample

Diagram 1.2 palm oil biodiesel

production using soxhlet.

Diagram 1.4 separation layer

ofbiodiesel and glycerin

40
 Diagram 1.7 for blended biodiesel

Diagram 1.5 biodiesel washing

Diagram 1.8 for cloud point test

Diagram 1.6 Intermediate glyceride

test

41