ABUBAKAR TAFAWA BALEWA UNIVERSITY

BAUCHI

PRODUCTION OF BIODIESEL FROM ZOBO (HIBISCUS

SABDARIFFA L.) SEED OIL

A PROJECT
SUBMITTED TO THE CHEMISTRY DEPARTMENT
SCHOOL OF SCIENCE AND SCIENCE TECHNOLOGY
ABUBAKAR TAFAWA BALEWA UNIVERSITY BAUCHI

IN PARTIAL FULFILMENT OF THE REQUIREMENT FOR THE AWARD

OF A BACHELOR OF TECHNOLOGY, B.TECH. (HONS) DEGREE IN
INDUSTRIAL CHEMISTRY

BY
ADULOJU ABIMBOLA
04/15281/1

SEPTEMBER 201I.

CERTIFICATION
This project titled "Production of biodiesel from Zobo (Hibiscus Sabdariffa L.) Seed Oil" was
conducted by Aduloju Abimbola O. (04/15281/1) and duly supervised and approved by Dr. I.Y
Chindo having met the requirement for the award of the degree of Bachelor of Technology in
Industrial Chemistry.

Dr. I.Y Chindo

(Supervisor)

Signature

Date

External Examiner

Signature

Date

Dr. H.M. Adamu

(Program Coordinator)

Signature

Date

DEDICATION
This thesis is dedicated to my parent for their timeless support throughout the course of my study
and for everything they have done in my life right from my childhood to this stage of my life.
Their support, parental love, care and advice were my driving force throughout my years of
academic study. Love you Dad and Mum.

ACKNOWLEDGEMENT
All thank is due to the Almighty, the Beneficent, the Merciful for sparing my life till this time.
I wish to start by acknowledging my mentor, my supervisor, and Uncle Dr. I.Y Chindo. I wish to
thank you sir for your constructive criticism, patience and understanding. May God continue to
guide and protect you and your family.
I also wish to acknowledge the following individuals who contributed immensely towards the
accomplishment of this work; Eleazar David, Ismail, Samson Olarinoye, Abdulrasheed
Abdulkareem and as much people that I cannot mention, I dont know how to thank you all for
your support. I pray to God Almighty to bless and reward you abundantly and increase you. To
my dear Deborah Adio, thank you for being there for me.

TABLE OF CONTENTS
CERTIFICATION ii
DEDICATION ..

iii

ACKNOWLEDGEMENT

iv

TABLE OF CONTENTS ..

LIST OF FIGURES ..

ix

LIST OF TABLES

ABSTRACT .. xi
CHAPTER ONE: INTRODUCTION
1.1.0 BRIEF HISTORY OF BIODIESEL ...

1.2.0 BIODIESEL: A TRANSESTERIFIED VEGETABLE OIL 2

1.2.1 IMPORTANCE OF BIODIESEL .

1.2.2 CAN BIODIESEL REPLACE PETRODIESEL? 4

1.3.0 FATS AND OILS 5
1.4.0 FATTY ACIDS

1.5.0 QUALITY PARAMETERS

1.6.0 LITERATURE REVIEW.10

1.6.1 HIBISCUS SABDARIFFA L. .....................................................10
1.6.2 THE FOOD USES AND VALUE OF ZOBO.11
1.7.0 AIM AND OBJECTIVES OF RESEARCH 12
CHAPTER TWO: MATERIALS AND METHODS
2.1.0 COLLECTION OF SAMPLES 13
2.2.0 SOLVENTS AND REAGENTS.. 13
2.3.0 MOISTURE CONTENT ... 13
5

2.4.0 n-HEXANE EXTRACTION

.14

2.5.0 PHYSICAL PROPERTIES OF OIL

.. 14

2.5.1 COLOUR

14

2.5.2 SMELL

. 15

2.5.3 TEXTURE . 15
2.5.4 SPECIFIC GRAVITY.15
2.5.5 VISCOSITY....15
2.5.6 DENSITY..16
2.6.0 CHEMICAL PROPERTIES OF OIL ..16
2.6.1 FREE FATTY ACID
2.6.2 ACID VALUE

. 16

17

2.6.3 PEROXIDE VALUE

. 17

2.6.4 SAPONIFICATION VALUE

18

2.6.5 IODINE VALUE ..

19

2.7.0 PREPARATION OF FATTY ACID METHYL ESTER

2.8.0 FUEL QUALITY PARAMETER TESTS

.20

21

2.8.1 FLASH PONT

..

21

2.8.2 POUR POINT

..

21

2.8.3 CLOUD POINT

..

22

2.8.4 DENSITY . 22
2.8.5 CALORIFIC VALUE

2.8.6 KINEMATIC VISCOSITY

2.8.7 CETANE NUMBER
2.8.8 FLAME TEST

23

.. 23

. 24

... 25

2.8.9 COMBINED GAS CHROMATOGRAPHY-MASS SPECTROMETRY

6

.25
2.9.0 PREPARATION OF REAGENTS
2.9.1 0.14M NaOH

. 25

25

2.9.2 GLACIAL ACETIC ACID/CHLOROFORM (3:2 V/V) .. 26

2.9.3 SATURATED POTASSIUM IODIDE 26
2.9.4 0.1N SODIUM THIOSULPHATE
2.9.5 0.5M HCl

..26

26

2.9.6 0.5M ETHANOLIC POTASSIUM HYDROXIDE .. 26

2.9.7 HANUS SOLUTION

2.9.8 15% POTASSIUM IODIDE

26
27

2.10.0 PREPARATION OF INDICATORS 27

2.10.1 1% STARCH INDICATOR

.. 27

2.10.2 PHENOLPHTHALEIN INDICATOR.... 27

CHAPTER THREE: RESULTS AND DISCUSSION

3.1

RESULTS ...

28

3.2

DISCUSSION

33

CHAPTER FOUR: CONCLUSION AND RECOMMENDATION

4.1

SUMMARY...35

4.2

CONCLUSION

4.3

RECOMMENDATIONS .. 37

. 36

LIST OF FIGURES
1. A TRYGLYCERIDE MOLECULE 2
2. THE MOLECULAR AND STRUCTURAL FORMULAE OF SOME
FATTY ACIDS
.. 6
3. ZOBO (HIBISCUS SABDARIFFA L.) ..... 10
4. SEPARATION OF BIODIESEL FROM GLYCEROL.
39

LIST OF TABLES

1. CHEMICAL NAMES AND DESCRIPTIONS OF SOME COMMON

FATTY ACIDS
. 6
2. MOISTURE CONTENT AND OIL RECOVERY OF HIBISCUS
SABDARIFFA L. SEED.............29
3. SMELL, COLOUR AND TEXTURE OF HIBISCUS SABDARIFFA L.
SEED OIL..
30
4. A COMPARISON OF OIL QUALITY PARAMETERS OF HSSO AND
THOSE OF CITRULLUS LANATUS SEED OIL AND CASTOR SEED
OIL 30
5. RESULTS OF THE FUEL QUALITY PARAMETERS OF HSSO,
CPFAMES AND D2
..40
6. COMPARISON OF THE RESULTS OF FUEL QUALITY PARAMETERS
OF HSFAMES WITH OTHER INVESTIGATED FAMES AND WITH
STANDARDS
. 45
7. GC-MS ANALYSIS OF BIODIESEL FROM HIBISCUS SABDARIFFA
L46

ABSTRACT
Due to the concern on the availability of recoverable fossil fuel reserves and the environmental
problems caused by the use of those fossil fuels, the global energy concern has led to the search
for alternative energy from the extensive consumption of fossil fuels. In this research the seed
oil of Zobo (Hibiscus sabdariffa L.) was investigated for its viability as a feedstock for
biodiesel production. The oil quality characteristics of the seed oil were; iodine value (IV), 39.46
g iodine/100g oil, peroxide value (PV), 26 meq peroxide/kg oil, acid value (AV), 16.50 mg
KOH/kg oil, saponification value (SV), 151.47 meqKOH/kg oil, free fatty acid (FFA), 8.29 % of
oil, specific gravity (S.G), 0.904 g/ml oil and viscosity, 29.13 mm2/s at 30 C. The oil was
9

transesterified using ethanol and potassium hydroxide and the parameters were compared to that
of petroleum diesel number 2 (D2). Fuel tests on the Hibiscus sabdariffa L. seed oil methyl ester
gave a high cetane number, 68.2 and a high flash point of 317 C. Other fuel properties of the
biodiesel assayed were cloud point, pour point, viscosity, density and calorific value and the
results were; -3 C, -19 C, 2.20 mm2/s, 871 kgm-3 and 124272 J respectively. The results
obtained for the biodiesel was also compared with the American and European standards for
biodiesel (ASTM D6751 and EN14214) and were found to fall within the acceptable limits,
implying that Hibiscus sabdariffa L. fatty acid ethyl ester could be used alone or as blends with
diesel D2 in diesel combustion engines in tropical regions like Nigeria. GC/MS analysis of the
ethylated oil revealed the presence of 4 ethyl ester (palmitoic ethyl ester, linoleic acid ethylester,
9-octadecenoic acid ethyl ester, and ethyl-octadecanoate).

10

CHAPTER ONE
1.0

INTRODUCTION

1.1.0 BRIEF HISTORY OF BIODIESEL

The concept of biodiesel dates back to 1885 when Dr. Rudolf Diesel built the first diesel engine
with the full intention of running it on vegetative sources (Knothe, 2001). He first displayed his
engine at the Paris show of 1900 and astounded everyone when he ran the patented engine on
any hydrocarbon fuel available which included gasoline and peanut oil (Knothe, 2001). In 1912
he stated"...... the use of vegetable oils for engine fuels may seem insignificant today. But such
oils may in the course of time become as important as petroleum and the coal tar products of
present time (Knothe, 2001). Since then, the requirements for an alternative internal combustion
engine fuel have grown increasingly. Whereas, in early years, it was sufficient for a fuel to
merely provide enough energy to gets the engine running. Now the fuel must also be non toxic,
biodegradable, come from renewable sources and minimize emissions of CO, NO x, unburned
hydrocarbons and CO2 (Ali and Hanna, 1994).
Today, the demand for alternative energy sources is frequent, because there is a progressive
decrease of the worlds petroleum (Knothe, 2001). Vegetable oil fuel or biodiesel is a potential
substitute for diesel fuel because it is made from renewable source (Ali and Hanna, 1994). In
addition, it can also be described as carbon neutral. This means that, the fuel produces no net
output of carbon in the form of CO 2 (Knothe, 2001). This effect occurs because when the oil crop
grows, it absorbs the same amount of CO 2 as it is released when the fuel is burnt (Knothe, 2001).
The American Society for Testing Material (ASTM) defines biodiesel as a fuel composed of

monoalkyl esters of long-chain fatty acids derived from renewable vegetable oils or animal fats
meeting the requirements of ASTM D6751(Canakci and Sanli, 2008).

1.2.0 BIODIESEL: A TRANSESTERIFIED VEGETABLE OIL

In simple terms, biodiesel is the product obtained when a vegetable oil or animal fat
(triglyceride) is chemically reacted with an alcohol to produce fatty acid alkyl esters in a process
called transesterification (Arjun, 2008). A catalyst such as sodium or potassium ethoxide or any
alkoxide is required, with glycerol produced as a co-product.
Chemically, most vegetable and animal oils and fats are triglycerides- glycerol bound to 3 fatty
acids, as shown in Figure 1below.
O

CH2

R1

CH

R2

CH2

R3

Figure 1: A triglyceride molecule

Where R1, R2 and R3 represent the hydrocarbon chains of the fatty acyl groups of the triglyceride.
It is this triglyceride that undergoes a chemical reaction breaking down and replacing the
glycerin portion with an alcohol molecule. The glycerin is then converted to glycerol and falls to
the bottom where it is drained off leaving the biodiesel. This will be explained in detail in
subsequent chapters.

Biodiesel is currently undergoing a phase of active research all over the world today. Researchers
at all levels are exploring the use of various plants as feedstock for biodiesel production. The
plants that have so far being investigated for this purpose in Nigeria and various parts of the
world include rapeseed, sunflower, jatropha, castor plant, soybean, thevitia, nerfolia etc (Arjun,
2008). The current research is therefore aimed at exploring the use of Hibiscus sabdariffa L seed
as a feedstock for biodiesel production.

1.2.1 IMPORTANCE OF BIODIESEL

There are five primary reasons why the development of biodiesel should be encouraged in
Nigeria as follows:
1. It provides a market for excess production of vegetable oils and animal fats.
2. It decreases the countrys dependence on petrodiesel (gasoline) which is currently being
imported.
3. It is renewable and does not contribute to global warming due to its closed carbon cycle.
4. The exhaust emissions (CO, unburned hydrocarbons, particulate emissions etc) from
biodiesel are lower than with fossil diesel.
5. Biodiesel has excellent lubricating properties than petrodiesel and hence reduces engine
wear.
In addition to these, biodiesel has some advantages over petrodiesel which include low toxicity,
superior flash point, biodegradability, negligible sulfur content etc (Knothe, 2001).
Consequently however, the production of biofuels has some disadvantages which include the
following;
1

Biodiesel take a large expanse of area to grow. As a result good land suitable for other
crops gets diverted to biofuel species (Holbrook, 2001).

Biofuels may raise the price of certain foods, which are also used for biofuel such as

3
4
5

corn.5
As other plants are replaced, soil erosion will grow (Holbrook, 2001).
A lot of water is used to water the plants, especially in dry climates (Holbrook, 2001).
Sometimes the production of some biofuels actually leads to more greenhouse gas
emissions than they decrease such as in the case of rapeseed corn etc (Holbrook, 2001).

1.2.2 CAN BIODIESEL REPLACE PETRODIESEL?

Despite the upsides, however, experts point out that biofuels are far from a cure for our
addiction to petroleum. A wholesale societal shift from gasoline to biofuels given the number
of gas-only cars already on the road and the lack of ethanol or biodiesel pumps at existing
filling stations, would take some time (Ali and Hanna, 1994).
Another major hurdle for widespread adoption of biofuels is the challenge of growing
enough crops to meet demand, something skeptics say might well require converting just
about all of the worlds remaining forests and open spaces over to agricultural land (Ali and
Hanna, 1994).
Replacing only five percent of the nations diesel consumption with biodiesel require
diverting approximately sixty percent of todays soya crops to diesel production, says
Mathew Brown, an energy consultant (Ali and Hanna, 1994).

1.3.0 FATS AND OILS

Fats and oils are primarily water- soluble, hydrophobic substances in the plant and animal
kingdom that are made up of one mole of glycerol and three moles of fatty acids and are

commonly referred to as triglycerides (Knothe, 2001).The properties of different fats and oils
depend upon the characteristics of the triglycerides of which they are mixtures and upon the
proportions of these triglycerides to one another (Knothe, 2001).Therefore, certain quality
tests has to be conducted on a fat or oil before being used for biodiesel production. Other
contaminants such as color and odor of bodies can in turn reduce the value of the glycerin
produced, and reduce the public acceptance of the fuel if the color and odor persist in the fuel
(Holbrook, 2001).

1.4.0 FATTY ACIDS

Fatty acids are component of both vegetable oil and biodiesel. They are ultimately consumed
in a wide variety of end use industries (rubber, plastics, detergents etc) (Canakci and Sanli,
2008).Fatty acids make up the greatest proportion of the current consumption of raw
materials in the chemical industry (Morton and Julia, 1987).
To describe precisely the structure of a fatty acid molecule, one must give the length of the
carbon chain (number of carbon), the number of double bonds and also the exact position of
these double bonds. Some common fatty acids usually found in most oils are shown in Table
1 below.

Table 1: Names and descriptions of some common fatty acids

Common Name
Butyric acid
Caprylic acid
Lauric acid
Myristic acid
Palmitic acid
Stearic acid
Oleic acid
Ricinoleic acid

Carbon
Atom
4
8
12
14
16
18
18
18

Double
Bonds
0
0
0
0
0
0
1
1

Linoleic acid

18

Gadoleic acid

20

Scientific Name

Sources

Butanoic acid
Octanoic acid
Dodecanoic acid
Tetradecanoic acid
Hexadecanoic acid
Octadecanoic acid
9-octadecenoic acid
12-hydroxy-9octadecenoic acid
9,12-octadecadieoic
acid

Butter fat
Coconut oil
Coconut oil
Palm kernel oil
Palm oil
Animal oil
Olive oil
Castor oil

9-eicosanoic acid

Peanut oil, fish oil

Grape seed oil

The molecular and structural formulae of some fatty acids are also shown in Figure 2 below.

OH
O

OH

BUTYRIC ACID

LINOLEIC ACID

(9, 12 -octadecadieoic acid)

PALMITIC ACID

Figure 2: The structures of some fatty acids

OH

(Hexadecanoic acid)

1.5.0 QUALITY PARAMETERS

CALORIFIC VALUE: Calorific value or heating value is the amount of heating energy released
by the combustion of a unit value of fuels (Alptekin and Canakci, 2009).One of the important
determinants of heating value is moisture content. Air-dried biomass typically has about 15-20 %
moisture, whereas the moisture content also affects the rate of biological activity on oils.
Therefore high moisture is not desirable (Alptekin and Canakci, 2009).
POUR POINT: This refers to the temperature at which the oil in solid form starts to pour
(Alptekin and Canakci, 2009). In cases where these temperatures fall below the melt point, the
entire fuel system including all fuel lines and fuel tank will need to be heated (Alptekin and
Canakci, 2009).
CLOUD POINT: The temperature at which oil starts to solidify is known as the cloud point
(Alptekin and Canakci, 2009). while operating an engine at temperatures below oils cloud point,
heating will be necessary in order to avoid waxing of the fuel (Alptekin and Canakci, 2009).
FLASH POINT: The flash point of a diesel fuel is the minimum temperature at which the fuel
will ignite (flash) on application of an ignition source (Alptekin and Canakci, 2009). Flash point
varies inversely with fuels volatility. Minimum flash point temperature of about 130 0Cis
required for proper safety and handling of diesel fuel (Alptekin and Canakci, 2009).
IODINE VALUE: This is the mass of iodine in grams that is consumed by 100g of a test
substance (Alptekin and Canakci, 2009). It is used in the determination of the amount of
unsaturation contained in fatty acids and other hydrocarbons. Many vegetable oils and some
animal fats are drying or semi drying and it is this which makes many oils such as linseed,
Tung and some fish oils suitable as the base for paints and other coatings (Alptekin and Canakci,

2009). But it is also this property that further restricts their use as fuels (Alptekin and Canakci,
2009).
VISCOSITY: Viscosity refers to the thickness of the oil, and it is determined by measuring the
amount of time taken for a given measure of oil to pass through an orifice of a specified size
(Alptekin and Canakci, 2009). Viscosity affects injector, lubrication and fuel atomization
(Alptekin and Canakci, 2009). Fuels with low viscosity may not provide sufficient lubrication for
the precision fit of the fuel injection pumps, resulting in leakage or increased wear (Alptekin and
Canakci, 2009).
PEROXIDE VALUE: Peroxide value is a measure of the peroxides contained in the oil. It is
used as a measure of the extent to which rancidity reactions have occurred in an oil or fat during
storage. The double bonds found in fats and oils play a role in autoxidation. Oils with a high
degree of unsaturation are more susceptible to autoxidation (a free radical reaction involving
oxygen that leads to deterioration of fats and oils which form off-flavors and off-odors)
(Alptekin and Canakci, 2009).
SAPONIFICATION VALUE: Saponification value represents the number of milligrams of
KOH or NaOH required to saponify1.0 g of fat under the conditions specified (Alptekin and
Canakci, 2009). It depends on the kind of fatty acids contained in the fat. This parameter is also
important in judging oil as it allows for comparison of the average fatty acid chain length
(Alptekin and Canakci, 2009).
ACID VALUE: This is the mass of KOH in milligrams required to neutralize the free fatty acids
present in 1.0g of the oil. The acid value is the measure of the extent to which the triglycerides in

the oil have been decomposed by lipase or other action. The decomposition is accelerated by heat
and light (Alptekin and Canakci, 2009).
CHROMATOGRAPHY: The term chromatography refers to a general method of separation in
which a mixture is partitioned between a stationary phase and a mobile phase. The moving phase
may be a vapor or a liquid, the stationary phase is a solid or liquid phase coated onto a solid
(Waheed and Zafar, 1980).
All the techniques depend on the same basic principle, that is variation in the rate which different
components of a mixture migrate through a stationary phase under the influence of the mobile
phase. The rate of migration varies because of difference in distribution ratios. Chromatography
now embraces variety of processes which are based on different distribution of sample
components between two phases; thermally stable volatile organic and inorganic compounds are
separated using Gas Chromatography as a technique of choice.

1.6.0 LITERATURE REVIEW

1.6.1 HIBISCUS SABDARIFFA L.
Hibiscus sabdariffa commonly referred to as Zobo in hausa, ishapa in Yoruba, belongs to
malvaceae family. It is an erect, mostly branched, annual shrub. Stems are reddish in color and
up to 3.5 m tall. Leaves are dark green to red, alternate, glabrous, long-petiolate, palmately
divided into 37 lobes, with serrate margins containing short-peduncles (Morton and Julia,
1987).

Figure 3: Hibiscus sabdariffa L.

Hibiscus has more than 300 species which are distributed in tropical and subtropical regions
around the world. (Morton and Julia, 1987). (Fig. 3), commonly named as red sorrel and
zobo Detailed studies on their use as a feedstock for biodiesel production are very limited,
especially in Nigeria.

1.6.2 THE FOOD USES AND VALUE OF ZOBO

Many parts of Hibiscus sabdariffa L. including the seeds, leaves, fruits and roots are used in
various foods. Among them, the fleshy red calyces are the most popular (Duke, 1983). They are
used fresh for making wine, juice, jam, jelly, syrup, gelatin, pudding, cakes, ice cream and
flavors and also dried and brewed into tea, spice, and used for butter, pies, sauces, tarts, and other
desserts (Duke, 1983). The calyces possess pectin that makes a firm jelly (Duke, 1983). The
young leaves and tender stems of zobo are eaten raw in salads or cooked as greens alone or in
combination with other vegetables and/or with meat (Duke, 1983). They are also added to curries
as seasoning. They have an acid, rhubarb-like flavor (Duke, 1983). The red calyces contain
antioxidants including flavonoids, gossypetine, hibiscetine and sabdaretine (Duke, 1983).
The fresh calyces are also rich in riboflavin, ascorbic acid, niacin, carotene, calcium, and iron
that are nutritionally important (Duke, 1983). The seeds, are high in protein, can be roasted and
ground into a powder then used in soups and sauces (Duke, 1983). The roasted seeds can be used
as a coffee substitute. The young roots are edible, but very fibrous (Duke, 1983).
1.6.3

MEDICINAL USES OF Hibiscus sabdariffa L.

Hibiscus sabdariffa L. is used in many folk medicines. It is valued for its mild laxative effect and
for its ability to increase urination, attributed to two diuretic ingredients, ascorbic acid and
glycolic acid (Watt and Breyer-Brandwijk, 1962). Because it contains citric acid, it is used as a
cooling herb, providing relief during hot weather by increasing the flow of blood to the skin's
surface and dilating the pores to cool the skin (Watt and Breyer-Brandwijk, 1962). The leaves
and flowers are used as a tonic tea for digestive and kidney functions (Watt and BreyerBrandwijk, 1962). The heated leaves are applied to cracks in the feet and on boils and ulcers to
speed maturation (Watt and Breyer-Brandwijk, 1962). The calyces and seeds are diuretic,

laxative and tonic (Watt and Breyer-Brandwijk, 1962). The ripe calyces, boiled in water, can be
used as a drink to treat bilious attacks (Duke, 1983). A lotion made from Hibiscus sabdariffa L.
leaves is used on sores and wounds (Watt and Breyer-Brandwijk, 1962).

1.7.0 AIM AND OBJECTIVES OF RESEARCH

1.7.1 AIM:
The aim of this research is to explore the use of transesterified Hibiscus sabdariffa L. seed oil as
a feedstock for biodiesel production.
1.7.2 OBJECTIVES:
The objectives of this research are:
i.
ii.
iii.

To carry out the extraction and transesterification of Hibiscus sabdariffa L. seed oil.
To carry out the physicochemical characterization of the oil and the resulting esters.
To compare the results of the esters with those of other investigated oils from literature
and with standards.

CHAPTER TWO

2.0

MATERIALS AND METHODS

2.1.0 COLLECTION OF SAMPLES

The Hibiscus sabdariffa L, (zobo) seeds were obtained from Muda Lawal market in Bauchi, and
were ground to powder in mortar in preparation for extraction.

2.2.0 SOLVENTS AND REAGENTS

The reagents used were of Analar grade obtained from a vendor of Eagle Scientific, BDH
chemicals limited Sigma-Aldrich Laboreh Chemikalein Gmbh, Germany.
The reagents and solvents include the following: starch, n-hexane, magnesium sulphate,
magnesium silicate, iodine, ethanol, phenolphthalein, glacial acetic acid, potassium iodide,
sodium thiosulphate, sodium hydroxide, hydrochloric acid etc.
The diesel D2 used as a control for the entire test was obtained from ATIL filling station,Yelwa
Bauchi.

2.3.0 MOISTURE CONTENT DETERMINATION

A small portion of the crushed Hibiscus sabdariffa L. Seed prepared for extraction was placed in
a dried and weighed crucible. The crucible with the sample was placed in a temperature
adjustable oven at 100 , heating and weighing at 50 mins intervals until the weight of the
sample remained constant. The crucible and its content were then allowed to cool, and the
moisture content determined using the formula shown below:

Percentage moisture =

WiWf
100
Wi

Where:
Wi = initial weight of sample (before drying)
Wf = final weight of sample (after drying).

2.4.0 n-HEXANE EXTRACTION

Using hot extraction, 80 g of the ground seed was loaded into a soxhlet extractor together with nhexane and the extraction carried out for 8 hours until it was certified that the oil was almost
completely extracted. The oil was then filtered using fluted Whatmann No.2 filter paper under
gravity to remove impurities such as anti bump granules, sand e.t.c present the hexane was
recovered using a rotary evaporator and the residual solvent evaporated in the fume cupboard.
The oil was weighed and the percentage oil recovery calculated on dry matter bases as shown
below;

Percentage recovery =

weig h t of oil
100
weig h t of sample on dry matter basis

2.5.0 PHYSICAL PROPERTIES OF OIL

32.5.1 COLOUR
The Hibiscus sabdariffa L. seed oil colour was determined by visual observation.
2.5.2

SMELL

The smell of the oil was identified by perceiving with the nose.

2.5.3

TEXTURE

The texture of the oil was determined by hand feeling.

2.5.4

SPECIFIC GRAVITY

An improvised specific gravity bottle was washed, rinsed with acetone and dried in the oven. The
bottle was cooled at room temperature in a desiccator and the weight of the empty bottle
determined using an electronic weighing balance. The weight of the bottle filled with water was
recorded. Then the water was poured out and the bottle was rinsed with acetone and dried in the
oven. The same procedure was repeated with the Hibiscus sabdariffa L. seed oil and the specific
gravity was computed as follows;

Specific gravity =

W 3W 2
W1

Where;
W3= weight of bottle + oil
W2= weight of empty bottle
W1= weight of equal volume of water

2.5.5

VISCOSITY

The viscosity of the Hibiscus sabdariffa L. seed oil was obtained using a viscometer. The oil was
filled to the mark on the viscometer, same as the water. The time of flow of the oil and the water
were determined using the equation below.
Viscousity = ts - tw
tw
Where; ts = time of flow of sample.
tw = time of flow of water.
2.5.6

DENSITY

The density of the Hibiscus sabdariffa L. seed oil was obtained by weighing a known volume
(17.6g) of the oil, where the density was determined using the equation below.
Density = W2 W1
V
Where; W2 = Weight of beaker and oil.
W1 = weight of empty beaker.
V = Volume of the oil.

2.6.0 CHEMICAL PROPERTIES OF OIL

2.6.1 FREE FATTY ACID (FFA)
Reagents
i.
ii.
iii.

Methanol
Phenolphthalein indicator
0.14 M NaOH

Procedure
The method used for the determination was that of the British standards institute no. 684
(AOAC, 1975).
A 1.0 g portion of the Hibiscus sabdariffa L. seed oil was placed in a 250 ml conical flask and
warmed. 25ml of methanol was added with thorough stirring, followed by 2 drops of
phenolphthalein indicator and a drop of 0.14 M NaOH solution. The contents were then titrated
with 0.14 M NaOH solution until a light pink color which persisted for 1 minute was observed.
The end point was recorded and used to calculate the FFA as shown below;

FFA (as oleic)

Titre M 28.2
weig h t of sample

Where;
M = Molarity of the base.
28.2 is a constant in calculation.

2.6.2 ACID VALUE (AV)

Reagents
i.
ii.
iii.

Methanol
Phenolphthalein indicator
0.14 M NaOH

Procedure
The method used for the determination was that of the British standards institute no. 684
(AOAC, 1975).
A 1.0 g portion of the Hibiscus sabdariffa L. seed oil was placed in a 250 ml conical flask and
warmed at 10oC. 25 ml of methanol was added while thoroughly stirring, followed by the
addition of 2 drops of phenolphthalein indicator and a drop of 0.14 M NaOH solution. The
contents were then titrated with 0.14 N NaOH solution until a light pink color, which persisted
for 1 minute was observed. The endpoint was recorded and used to calculate the acid value as
shown below;
Acid value = % FFA (as oleic) x 1.99

2.6.3 PEROXIDE VALUE (PV)

Reagents
i.
ii.
iii.
iv.

Saturated potassium iodide solution

Glacial acetic acid
Chloroform
0.1 N Sodium thiosulphate

Procedure
The method used was that of the British standards institute no. 684 (AOAC, 1975).

A 1.0 g portion of the Hibiscus sabdariffa L. seed oil was placed in a 250 ml conical flask and 30
ml glacial acetic acid/chloroform (3:2 V/V) was added. The contents were shaken until they
dissolved. 1.0 ml of saturated potassium iodide was added followed by the addition of 0.5 ml
starch indicator. This was titrated with 0.1 N Na2S2O3 until the dark blue color just disappeared.
Blank determination was also carried out and the peroxide value calculated as shown below;

PV (mEq/kg oil)

( SB ) 1000 N
W

Where;
S= titre volume of sample
B= titre volume of blank
N= normality of sodium thiosulphate solution
W= weight of oil sample

2.6.4 SAPONIFICATION VALUE (SV)

Reagents
i.
ii.
iii.

0.5 M hydrochloric acid

Ethanol potassium hydroxide solution (0.5 M in 9 5 % ethanol)
Phenolphthalein indicator

Procedure
The method used was that of the British standards institute 1995 (AOAC, 1975).
A 1.0 g portion of Hibiscus sabdariffa L. seed oil was placed in a 250 ml conical flask and 25 ml
of 0.5 M ethanol potassium hydroxide solution was added.
A reflux condenser was attached and the flask content refluxed for 30 minutes on a water bath at
30oC while swirling until it simmered. The mixture was then titrated against 0.5 M HCl using

phenolphthalein indicator while still hot. A blank determination was also carried out under the
same conditions and the saponification value calculated as shown below;

SV =

( BS ) 28.05
W

Where;
B = titre value of blank
S = titre value of sample
W = weight of oil

2.6.5 IODINE VALUE (IV)

Reagents
i.
ii.
iii.
iv.
v.

Anhydrous chloroform
Hanus solution
15 % potassium iodide
0.1 N sodium thiosulphate
1.0 % starch indicator

Procedure
Several methods are available for iodine value determination but Hanus method (Association of
Analytical Chemist.1975) was used in this work (AOAC, 1975).
A 1.0 g portion of Hibiscus sabdariffa L. seed oil was placed in a 250 ml conical flask followed
by 30 ml Hanus solution and the flask stopped. The flask content was mixed and kept in the
drawer for 30 mins. It was then titrated against 0.1 N Na 2S2O3 until the solution became light
yellow. 2.0 ml of 1.0 % starch indicator was added and the titration continued until the blue color
just disappeared. A blank determination was also carried out under the same conditions and the
IV calculated as thus;

IV =

( BS ) 12.69 N
W

Where;
B= blank titre
S= sample titre
N= normality of Na2S2O3
W= weight of oil
12.69 is a constant in the calculation.

2.7.0 PREPARATION OF FATTY ACID METHYL ESTER (FAMES)

Reagents
i.
ii.
iii.
iv.

5 ml of 95 % methanol
0.3 g KOH
15 ml CPSO
Anhydrous MgSO4

Procedure
The method used was that developed by the biodiesel team (AOAC, 1975). Methanol (10 ml)
was added to KOH (0.3 g) in a conical flask with slight heating at 30 oC and slow stirring until
complete dissolution was achieved.
The alcoholic KOH was added to 15 ml of Hibiscus sabdariffa L. seed oil while it was stirring
slowly and heating at 30oC. The speed of the stirring was increase and allow to stir for few hours
until sign of separation was identified. The mixture was then slowly transferred to a separating
funnel and allowed to stand for 1 hour. Two layers became distinct and the glycerol layer (the
lower layer) was drained off. Magnesium silicate was added to the FAMES, swirled and allowed
to settle down in the separating funnel after which it was run off. This washing process was
repeated until the product was moisture free. The yield was calculated as shown below;

% yield of biodiesel

weig h t of biodiesel
100
weig h t of Hibiscus sabdariffa seed oil

2.8.0 FUEL QUALITY PARAMETER TESTS

2.8.1 FLASH POINT (FP)
Apparatus
i.
ii.
iii.

Thermometer (reading in )
100 ml conical flask
Hot plate

Procedure
An improvised method was used for this determination. A 5 ml portion of the biodiesel was
poured into a test tube set on a clamp and a hot plate, it was then heated at slow constant rate
(specify rate) on the hot plate. The flash point was taken at the lowest temperature when an
application of the test flame caused the vapor above the sample to ignite. This was also carried
out for the control, diesel D2 and the test sample, Hibiscus sabdariffa L. seed oil.
2.8.2 POUR POINT (PP)
Apparatus
i.
ii.
iii.
iv.

Thermometer (reading in )
Cylindrical test tube
Ice bath
Clamp stand

Procedure
An improvised method was used for this determination (Abayeh and Ugah, 2007).
The cylindrical test tube was filled with the biodiesel to the 5.0 ml mark and clamped with a
wooden clamp bearing a thermometer. The sample was then allowed to cool below 0 in the
ice/salt bath. At this point it was removed and tilted on the clamp and the set up observed at

intervals. The lowest temperature at which the biodiesel was observed to flow was recorded as
the pour point. The same procedure was repeated for diesel fuel, D2.
2.8.3 CLOUD POINT (CP)
Apparatus
i.
ii.
iii.
iv.

Thermometer (reading in )
Cylindrical test tube
Ice bath
Clamp stand

Procedure
An improvised method was used for this determination (Abayeh and Ugah, 2007).
The cylindrical test tube was filled with the biodiesel to the 5.0 ml mark and clamped with a
wooden clamp bearing a thermometer. The test tube was placed in the ice/salt bath and the set up
inspected at intervals for cloud formation. The temperature at which a distinct cloudiness was
observed to appear at the bottom of the test tube was recorded as the cloud point of the biodiesel.
The test was carried out for Hibiscus sabdariffa L. seed oil and diesel D2.
2.8.4 DENSITY
Apparatus
i.
ii.

Beaker
Electronic weighing balance

Procedure
The weight of a small empty bottle was determined using an electronic weighing balance. The
bottle was then filled to the brim with the biodiesel and the weight of the bottle and the biodiesel

determined. This procedure was repeated with the diesel D2, and the density was calculated
using the formula shown below:
W 2W 1
Density () =
V

Where;
W2

=Weight of bottle + Sample

W1

=Weight of empty bottle

V=Volume of Sample
2.8.5 CALORIFIC VALUE (CV)
Apparatus
i.
ii.
iii.
iv.
v.

Burner (a locally made lamp)

Beaker(100 ml)
Wick
Thermometer (reading in o C)
Stop Clock

Procedure
An improvised method was used for this determination (Abayeh and Ugah, 2007).
The wick was positioned in the locally made lamp. The weight of the empty lamp with 10 ml of
the biodiesel was taken. The wick was lit and the biodiesel was used to heat the beaker
containing 10 ml of water for 10 minutes after which the temperature of the water was recorded.
The same procedure was repeated for diesel D2 and the calorific value/content determined using
the formula
Calorific value = MC

Where;
M = Mass of water
C = Specific heat capacity of water
= Temperature rise of water after 10minutes

2.8.6 KINEMATIC VISCOSITY

Apparatus
i.
ii.
iii.
iv.

U-tube Viscometer
Pipette filler
Thermometer
1.0L measuring cylinder

Procedure
The viscometer was placed in the 1.0L measuring cylinder filled to mark with water and
regulated to the appropriate temperature. The tube was then filled up to a graduation mark over
the left storage bulb with the biodiesel. The biodiesel was then sucked up to fill the higher
storage bulb in the right left of the tube and then released. The time taken for the biodiesel to
flow from the upper mark to the lower was observed and calculated. The kinematic viscosity of
the biodiesel calculated using the formula below:

Kinematic viscosity () =

Absolute Viscosity () =

Absolute Viscosity()
Density ()
t

Where;
t = time of flow of the sample
t0 = time of flow of the reference (water in this case)

The same procedure was repeated using diesel D2 and water, which was taken as the
reference.

2.8.7 CETANE NUMBER (CN)

The parameter was determined based on the formula proposed by Demirbas 1998 as there was no
enough biodiesel to carry out the test. The formula is given below

CN =

46.3+

5458
0.225 IV
SV

Where;
SV =Saponification value of the oil
IV =Iodine value of the oil
2.8.8 FLAME TEST
Apparatus
i.
ii.
iii.

Wick
Watch glass
Test tube

Procedure
The wick was dipped in the test tube containing 5.0 ml of the biodiesel and then placed on a
watch glass. The wick was then lit and allowed to burn. The rate of burning, the color of the
flame werecolor of the flame was noted and recorded. The same procedure was repeated using
diesel D2.
2.8.9

COMBINED GAS CHROMATOGRAPHY-MASS SPECTROMETRY

The components of the ethylated oil were identified by a combined gas chromatography-mass
spectrometry (GC-MS) using GCMS-QP 2010 Shimadzu, Japan carried out at NARICT, Zaria.

This was achieved by injecting 8L into a GCMS interfaced to a computer library search. The
GC column oven temperature (70oC, injecting temperature (250oC), flow control mode (linear
velocity), total flow (40.8 mL/min) column flow (1.80 mL/min), pressure (116.9 kpa), linear
velocity (49.2 cm/sec), purge flow (3.0 mL/min), and split ratio (20.0) were employed for this
analysis

2.9.0 PREPARATION OF REAGENTS

2.9.1 Preparation of 0.14 M NaOH
NaOH (1.4 g) was dissolved in a small quantity of distilled water and the solution transferred
into a 250 ml volumetric flask and made to the mark with distilled water.
2.9.2 Preparation of glacial acetic acid/chloroform (3:2 V/V) solution
Glacial acetic acid (150 ml) ad chloroform (100 ml) was mixed in a 250 ml volumetric flask and
the resultant solution kept for use.
2.9.3 Preparation of saturated potassium iodide solution
Excess potassium iodide was dissolved in a 250 ml volumetric flask containing distilled water
until it was ensured that the crystal no longer dissolves.

2.9.4 Preparation of 0.1 N sodium thiosulphate solution

Sodium thiosulphate (1.98 g) was dissolved in a small quantity of distilled water. It was then
transferred into a 250 ml volumetric flask and made to the mark with distilled water.
2.9.5 Preparation of 0.5 M HCl
Concentrated HCl (10.8 ml) was measured into a 250 ml volumetric flask containing some
quantity of distilled water and was made up to the mark with distilled water.
2.9.6 Preparation of 0.5 M ethanolic potassium hydroxide solution
KOH (10 g) was weighed, dissolved in a small quantity of 95 % ethanol and made up to the mark
with 95 % ethanol in a 250 ml volumetric flask.
2.9.7 Preparation of Hanus solution
Iodine (3.3 g) was dissolved in a small quantity of glacial acetic acid and made up in a 250 ml
volumetric flask with glacial acetic acid. The solution was heated on a hot plate and stored in a
brown stoppered bottle in the dark.
2.9.8 Preparation of 15 % potassium iodide solution
Potassium iodide (15 g) was dissolved in a small quantity of distilled water and made up to the
mark in a 100 ml volumetric flask with distilled water.

2.10.0 PREPARATION OF INDICATORS

2.10.1 Preparation of 1% starch indicator solution
Soluble starch (1.0 g) was weighed and mixed with water in 100 ml beaker and warmed water
(50 ml) was added while stirring. The solution was heated until a clear solution resulted. It was
then made to the 100 ml mark with water, allowed to cool and used immediately.

2.10.2 Preparation of phenolphthalein indicator

Phenolphthalein (1.0 g) was weighed and dissolved in 100 ml of absolute alcohol.

CHAPTER THREE
3.0 RESULTS AND DISCUSSION
3.1 RESULTS
Results for the moisture content of three different samples of Hibiscus sabdariffa L. seed sample
is shown in Table 2.
Table 2: Moisture content and oil recovery of Hibiscus sabdariffa L. seed
Weight of sample
before drying(g)
5.8
5.9
5.7

Weight of sample Percentage moisture

after drying(g)
(%)
5.5
5.5
5.7

5.17
6.70
5.17

The result of the moisture content of the three different samples all fall within the long period of
(5-7 %) moisture content. The percentage oil content (12.83%) is low as shown in Table 4.

The results of the odour, color and texture of Hibiscus sabdariffa L. seed oil is presented on table
3. A comparison of oil quality parameters of Hibiscus sabdariffa L seed oil with those of
Citrullus lanatus seed oil and castor seed oil presented in Table 4.
Table 3: Odour, color and texture of Hibiscus sabdariffa L. oil
Extract (sample)
A
B
C

Odour
Pleasant
Pleasant
Pleasant

Color
Darkish-brown
Darkish-brown
Darkish-brown

Texture
Viscous
Viscous
Viscous

Table 4: A comparison of oil quality parameters of Hibiscus sabdariffa L. and those of

Citrullus lanatus seed oil and castor seed oil.
Parameters

Hibiscus
sabdariffa L. seed
oil

Citrullus lanatus
seed oil (CLSO)

Castor seed oil

(CSO)

Moisture %
Oil recovery %
Color
Odor
Specific gravity g/ml
Viscosity mm2/s
Density g/ml
Acid value mgKOH/g oil
Peroxide Vale meq/kg
Iodine value g/100g
Saponification value
meq/kg
Free fatty acid %

5.68
12.83
Darkish-brown
Pleasant
0.904
30, 29.13
0.967
16.50
26
39.46
151.47
8.29

4.91
43.32
Yellow-brown
Pleasant
0.860
40, 10.73
N.A
0.50
18.75
58.42
115.94
N.A

4.15
33.20
Amber
N.A
0.960
28, 9.4247
N.A
1.148
N.A
87.72
175-187
N.A

N.A = Not Available

Fig. 5: Separation of biodiesel from glycerol.

The biodiesel yield was worked out to be 33.3%, this is extremely low, However, it still fall
within the requirement for the yield of biodiesel in oil which is 20 % of the oil.
Prior to use as a commercial fuel, the biodiesel must be analyzed in the laboratory to ensure that
it meets the ASTM specifications. The results of some of these parameters that were analyzed are
shown in Table 5 below. Comparison of the results of fuel quality parameters of HS FAEES with
other investigated FAEES and with standards is shown in Table 6.

Table 5: Results of the fuel quality parameters of Hibiscus sabdariffa L., and D2
Fuel properties
Kinematic viscosity (30),
mm2/s
Density, kgm-3
Flash point, C
Cloud point, C
Pour point, C

Hibiscus
sabdariffa L.
33.44

D2

871
317
-3
-19
73.45

835
140
0
-2

2.65

12472
Burns slowly with
A dark and thick
smoky flame

Cetane number*
Calorific value, J
Flame test

12188
Burns vigorously
with a dark and
thick smoky flame

*CN = 46.3 + 5458/SV -0.225 IV. Source (Demirbas, 1998.)

Table 6: Comparison of the results of fuel quality parameters of HS FAEES with other
investigated FAEES and with standards
Parameter

HS
FAEES

TN
FAEES

S
FAEES

D2

Density, g/cm3
Kinematic
viscosity, mm2/s
Flash point, C
Cloud point, C
Pour point, C
Calorific value, J
Cetane number*

0.8710
33.44

0.8811
3.00

0.8845
5.75

0.8350
2.65

317
-3
-19
12472
73.45

120
7.7
-3.8
16204
NA

168
-5
NA
NA
56

140
0
NA
12188
-

ASTM
D6751
Limits
0.8200 min
1.9-6.0

EN
14214
limits
0.86-0.9
3.5-5.0

130min
NA
NA
NA
47min

>101
NA
NA
NA
51min

*Demirbas 1998 min = minimum

HSFAEES= Hibiscus sabdariffa L. seed fatty acid ethyl ester
TNFAEES=Thevitia nerifolia fatty acid ethyl ester
SFAEES= Soybean fatty acid ethyl ester
D2=Diesel fuel
N.A= Not Available

The result of fuel properties of ethyl esters of Hibiscus sabdariffa L. seed oil are compared with
soy oil and Thevitia nerifolia ethyl esters, diesel fuel, ASTM D6751 and EN 14214 standards in
Table 6.
Table 7 shows the GC-MS analysis result of the biodiesel from Hibiscus sabdariffa L.

Table 7: GC-MS ANALYSIS OF BIODIESEL FROM HIBISCUS SABDARIFFA L.

Peak no.

Retention
time (mins)

16.017

%
peak
Area
22.16

%
Masses of fragment ions (M/Z) (% abundance). Proposed Identity
peak
height
25.63 88(100),101(50),55(20),57(18),284(18),70(17),24 Palmitic acid, ethyl ester
(Hexadecanoic ethyl ester).
1 (15),239(12),213(5),115(M+,3)

17.558

37.55

31.83

81(100),67(90),95(80),55(60),41(45),109(30),262
(25),308(15),123(12),121(12),135(10),164(5),178
(4),220(M+,3)

Linoleic acid, ethyl ester (9,12octadecadienoic acid ethyl

ester).

17.633

37.51

31.50

55(100),69(65),83(61),88(60),97(55),98(45),43(4
5),
101(41),57(35),264(25),266(18),222(17),123(13),
180(10),310(M+,10)

9-octadecenoic acid, ethyl ester

(E)-9-octadecenoic acid ethyl
ester).

17.851

5.94

7.41

88(100),101(55),43(40),55(28),55(28),57(22),70( Ethyl n-octadecanoate

17),89(12),312(12),269(11),213(10),115(8),60(M+ (octadecanoic acid, ethyl
ester).
,5)

19.007

2.84

3.63
55(100),41(88),81(71),67(70),69(42),83(37),68(3
6),95(35),79(34),99(25),121(M+, 15)

unknown

From the table, it can be observed that the retention time from peak no. 1 to peak no. 5 steadily increase from 16.017-19.007 min. The
proposed identities of the components shows the presence of ethyl ester, but the last component does not show any semblance to the
identities in the GC-MS library.

3.2

DISCUSSION

From Table 2, it can be observed that the moisture content of Hibiscus sabdariffa L. seed (5.17
%) is quite high compared to those of Citrullus lanatus seed oil (4.91%) and castor seed oil (4.15
%) but shows that the seed is within the range (5-7%) of the long term storage period seed,
implying that the seed can be stored for a long time without deteriorating.
The average oil recovery of Hibiscus sabdariffa L. seed oil (12.8 %) which is quite low as
compared to those of Citrullus lanatus and castor seed oil (Table 4). This would be a great
disadvantage in the use of Hibiscus sabdariffa L. compared to other oils with respect to the oil
price and the oil yield. The oil recovery for Hibiscus sabdariffa L. (12.83%) is low compared to
Citrullus lanatus seed oil (43.32) and Castor seed oil (32.20). The oil was observed to be
odourless, this is one of the qualities required of a good commercial oil. The free fatty acid (FFA)
value normally indicates the condition of the oil. It is often calculated as oleic acid because
British Standards Institute expresses it as the most abundandant acid in the oil. The FFA value
obtained for Hibiscus sabdariffa L. (8.29%) as compared to NAFDAC standard (6.0%) is high
and therefore, does not support good value as edible oil. (Christie, 1982). The specific gravity of
Hibiscus sabdariffa L.oil as obtained was 0.904. this falls within the value 0.89-0.92 reported for
edible oil (Odufoye, 1998).The acid value, peroxide value, saponification value, and the iodine
value are obtained as 16.50, 26, 151.47, and 39.46 respectively, the implication of these values
are that the oil will require acid pretreatment because of its high acid value, it could easily
become rancid because of its high peroxide value. The biodiesel properties such as; kinematic
viscousity (33.44 mm2/s), density (871 kgm-3), flash point (317 oC), cloud point (-3oC), pour
point (-19oC), cetane number (73.45), calorific value (12472 J), all fall within acceptable values
for biodiesel production.

The GC/MS analysis performed on the ethylated oil revealed that most of the free fatty acids
(FFA) were successfully ethylated except for component 5 (unknown identity) with retention
time of 19.007 min. from the summary of the GCMS analysis for Hibiscus Sabdariffa L.
ethylated oil, the following fatty acid esters identities are proposed:
Component 1 with retention time of 16.017 min (base peak) may be palmitoic ethyl ester,
component 2 with retention time of 17.558 min (base peak) may be linoleic acid ethyl ester,
component 3 with retention time of 17.633min (base peak) may be 9-octdecenoic acid ethyl
ester, componetnt 4 with retention time of 17.851min (base peak) may be ethyl n-octadecanoate,
component 5 with retention time of 19.007 is unknown.

CHAPTER FOUR
4.1
4.2

SUMMARY, CONCLUSION AND RECOMMENDATION

SUMMARY

In this work, the seed oil of Zobo (Hibiscus sabdariffa L.) was evaluated for the first time for
its viability as a feedstock for biodiesel production. The oil quality characteristics of the seed oil
were; iodine value (IV), 39.46 g iodine/100g oil, peroxide value (PV), 26 meq peroxide/kg oil,
acid value (AV), 16.50 mg KOH/kg oil, saponification value (SV), 151.47 meqKOH/kg oil, free
fatty acid (FFA), 8.29 % of oil, specific gravity (S.G), 0.904 g/ml oil and viscosity, 29.13 mm 2/s
at 30 C. The oil was transesterified using ethanol and potassium hydroxide and the parameters
were compared to that of petroleum diesel number 2 (D2). Fuel tests on the Hibiscus sabdariffa
L. seed oil methyl ester gave a high cetane number, 68.2 and a high flash point of 317 C. Other
fuel properties of the biodiesel assayed were cloud point, pour point, viscosity, density and
calorific value and the results were; -3 C, -19 C, 2.20 mm 2/s, 871 kgm-3 and 124272 J

respectively. The results obtained for the biodiesel was also compared with the American and
European standards for biodiesel (ASTM D6751 and EN14214) and were found to fall within the
acceptable limits, implying that Hibiscus sabdariffa L. fatty acid ethyl ester could be used alone
or as blends with diesel D2 in diesel combustion engines in tropical regions like Nigeria. GC/MS
analysis of the ethylated oil revealed the presence of 4 ethyl ester (palmitoic ethyl ester, linoleic
acid ethylester, 9-octadecenoic acid ethyl ester, and ethyl-octadecanoate).
4.2

CONCLUSION

The preliminary investigation indicates that Hibiscus sabdariffa L. seed oil is an economically
non-viable oil source because of its low oil content (12.83%). The oil quality parameters shows
that the oil is composed of moderately long chain fatty acids with a moderate degree of
unsaturation, thus low susceptibility to oxidative rancidity making it a good feedstock for
biodiesel production.
After transesterification which yielded 33.3 wt % biodiesel, the fuel quality parameters of the
FAEES also indicates that the fuel can be used in tropical regions like Nigeria. It has high flash
point making it free from fire hazards associated with fuel during storage and transportation. All
of the tested fuel quality parameters conform to standards for biodiesel fuels. The result of the
flame test also showed the advantage biodiesel has over petrodiesel as it shows a relative
decrease in the emission of greenhouse gases especially associated with petrodiesel.
In conclusion, from all the results obtained in this research, it was seen that Hibiscus sabdariffa
L. seed can serve as a good feedstock for biodiesel production. It was also seen that the resultant
fatty acid methyl ester can be used alone in diesel engines or as blends with petrodiesel as it
satisfies all the fuel quality parameters tested.

4.3

RECOMMENDATIONS

The result obtained in this research provides some important information that could be exploited
for potential use of the seed oil in biodiesel production. It is therefore recommended that further
researches be carried out to determine if the ethyl ester could also be used in diesel engines or as
blends with petrodiesel.
It is also recommended that researches be diversified in the field of biodiesel production. Nigeria
today is blessed with a variety of plants both edible and non edible which has not been exploited.
Therefore researchers should intensify their efforts in exploring the use of these plants as this
will reduce the nations dependence on petrodiesel and provide job opportunities in the labour
market.

REFERENCES
A. Demirbas. (1998). Fuel Properties and Calculation of Higher Heating Values of Vegetable
Oil. Fuel Energy Policy, 77:1117-20.

Association of Official Analytical Chemists, (AOAC, 1975). Official Methods of Analysis,

12th ed. Washington D.C. pp581-596.
B.C. Arjun. (2008). Non-edible Plant Oils as New Sources for Biodiesel Production. Int.
Journal of molecular sciences. ISSN 1422-0067. 9:169-180
C. L. Peterson; H. Haines and C. Chase. (1993). Rapeseed and Safflower oils as diesel fuels.
First Biomass Conference of the Americas: Energy, Environment, Agriculture and
Industry. Aug. 30 September. Burtington, Vermont pp33-40.
E. Alptekin and M. Canakci. (2009). Characterization of the Key Fuel Properties of Methyl
ester-diesel Fuel Blends. Fuels, 88:75-80.
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