CHAPTER ONE

INTRODUCTION

1.0 Background to the study

Despite the renewability and low toxicity advantages of vegetable oils over mineral oils, their
high processing costs, lower their market demands, hence the need to optimize their parent
reactions for improved cost competition. Bio-lube was produced from fuel oil via enzymatic
esterification in a solvent–free system. The tribological and physico-chemical properties of the
lube oil proved it to be biodegradable and environmentally friendly, although, the enzymatic
esterification process was noted to be quite complex and expensive. (Belafi, et al, 2019).

Transesterification is the reaction between an alcohol (Methanol/ethanol) and triglyceride in the

presence of a catalyst for the production of methylester which can subsequently be converted to
lube oil; an alkali catalyst usually makes the reaction faster compared to other catalysts. About
85-90 % of the total global lubricants are obtained from non-renewable petroleum precursors
/mineral oils. The continuous and conscious exploration of cheaper means of conversion of
polyolesters sourced from fatty acids of vegetable oils may result in significant cost reduction of
the synthesized lube oil. (Erhan et al, 2018)

In the study carried out by Ghazi et al., the kinetics of the transesterification synthesis of bio-
lubricants from Cassia tora oil was done at varying temperatures and constant pressure. Their
findings showed that the highest lube oil yield (i.e. 47 %) was obtained at 200 °C. A good
lubricant is characterized by properties such as its ability to resist wear, low freezing point, high
viscosity index, thermal stability, specific heat capacity, boiling points and high resistance to
oxidation and corrosion. Based on the study of (Ghazi et. Al, 2019).

Harnessing the potentials of exploiting green technologies for biodiesel production is a necessity;
although, the target product is bio lubricant, the study shows that the stages of bio lubricant
production can be optimized. A lubricant controls friction for improved efficiency and reduced
wear in automobiles and machine parts, whereas, bio-lubricant serves as fuel for automobiles.
(Helwani et al,2019).

1
The re-esterification process involved a high free fatty acid oils for improved bio lubricant yield.
Bio-lubes are valuable alternatives to petroleum-sourced lubricants due to their renewable nature
and lesser pollution effects with respect to their release of toxic substances. Their fuel properties
are somewhat comparable, which corroborates the need to improve on the quality and cost of
lube oils synthesized from vegetable oils. In addition, research on the use of biofuels as
replacements for fossil fuels has grown significantly because, fossil fuels are known to have high
quantity of gaseous emissions which may result in climate change, drought and threat to plant
and animal existence. (Kombe, 2018).

Transesterification reaction is usually between an alcohol (Methanol/ethanol) and triglyceride in

the presence of a catalyst. In a base-catalyzed transesterification process, the FFAs and percent
moisture are to be controlled as they result in side-reactions such as hydrolysis and
saponification thus, it is therefore recommended that the FFA value be less than 3% in order to
allow for maximum conversion.

Increased in acidity decreases the efficiency of conversion of TAGs to esters. Oziokwo carried
out extraction and characterization of lube oil obtained from sunflower oil and the lube oil
produced was seen to have similar properties with those of light duty oil (SAE) and heavy duty
oil (SAE40) with good flash/fire points in the range of 243 °C-290 °C and 260 °C-300 °C
respectively. (Meher et al, 2018).

1.2 Statement of the Problem

i. Not much work has been done regarding the development of biolubricant production
from sunflower and cassia tora blended oils.
1.3 Aim of this research project
The aim of this research work is to characterize and optimize the biolubricant production from
sunflower and cassia tora blended oil using response surface methodology.
The aim can be achieved through the following objectives.

1.4 The Objectives Of The Research Study.

i. To characterize sunflower and cassia tora blended oil

ii. To produce biolubricant from blended oil of cassia tora and sunflower.

2
 iii. To optimize the production of the bio lubricant from the blended oil through
experimental design.
iv. To compare the properties of biolubricant produced with the properties of conventional
lubricant

1.5 Scope

i. Within the scope of this research work, is the production of biolubricant from sunflower
and cassia tora blended oil using response surface methodology.
ii. To optimize the production of the biolubricant through experimental design.

1.6 Justification

Upon The completion of this project, the following will be achieved.

i. The outcome will educate on how to characterize and optimize the production of bio
lubricant from sunflower and cassia tora blended oil using experimental design.
ii. It will also result in having a final product with a good physio chemical property when
compared with conventional lubricant.

1.7 Definition of Terms and Terminologies

i. Optimization: this has to do with the design and operation of a system or process by
transforming it into a defined sense. Or it has to do with the use of a specific method to
determine the most cost effective and efficient solution to a problem or design for a
process.
ii. Lubrication/Lubricant: Lubrication occurs when two surfaces are separated by a
lubricant film. A lubricant is a liquid substance introduced between two moving surfaces
to reduce friction, wears and tears, and to improve efficiency of the moving part.
iii. Bio lubricant: is a renewable mixture of liquid substance obtained from edible and non-
edible seeds, vegetable oil or animal oil applied between two moving surfaces to reduce
friction, Wear and tears and to improve efficiency of the moving part.

3
 CHAPTER TWO

LITERATURE REVIEW

2.1 Cassia Tora Plant

2.1.1 Description

The Cassia tora is an herbaceous annual fetid herb. The plant can grow 30–90 centimeters (12–
35 in) tall and consists of alternative pinnate leaves with leaflets mostly with three opposite pairs
that are obovate in shape with a rounded tip. The leaves grow up to 3–4.5 centimeters long. The
stems have distinct smelling foliage when young. The flowers occur in pairs in axils of leaves
with five petals and pale yellow in colour. The stamens are of unequal length. The pods are
somewhat flattened or four angled, 10–15 cm long and sickle shaped, hence the common name
sickle pod. There are 30–50 seeds within a pod. ( Eriola,2013).

2.1.2 Growing conditions

Cassia tora is considered an annual weed, is very stress tolerant, and is easily grown. In Nigeria,
it occurs as a wasteland rainy season weed and its usual flowering time is after the monsoon
rains, during the period of October to February. Cassia tora grows in dry soil from sea level up to
1800 meters. The seed can remain viable for up to twenty years. Up to 1000 plants can emerge
per square meter following rain. Once the seed has matured, it is gathered and dried in the sun. In
Nigeria, it usually dies off in the dry season of July–October. (Eriola et al, 2013).
2.1.3 Cultivation

Soak the seeds for 2–3 hours in warm water before sowing it from early spring to early summer
in a warm greenhouse or pot in your own home. The seed usually germinates in 1–12 weeks at
23°C. Cassia tora can be transplanted. (Myers, 2014).

4
2.1.4 Pests/diseases of cassia tora

Mostly in Northern Nigeria were the availability of this plant is, Cassia tora has been known to
suffer limited damage by the leaf-eating larvae of a species of moth called Stegasta variana , a
Gelechild moth. (Prerna, 2012).

5
  GALLARY

Fig 2.1 Cassia tora seeds/ Cassia Tora plant.

1.2.5 Uses of cassia tora seeds

Cassia tora has many uses. The whole plant and roots, leaves, and seeds have been widely used
in traditional Indian and South Asian medicine. The plant and seeds are sometimes edible.
Young leaves can be cooked as a vegetable while the roasted seeds are used as a substitute
coffee. In Sri Lanka, the flowers are added to food. It is used as a natural pesticide in organic
farms, and as a powder commonly used in the pet food industry. (Putnam et al,2018).

6
2.2 Sunflower Plant

2.2.1 GALLARY

Fig 2.2 Sunflower plant/Sunflower seeds.

2.2.3 Description

Sunflower, (Helianthus annulus,) is an herbaceous annual plant in the family Asteraceae, grown

for its seeds. The plant has a thick, hairy, erect stem which gives rise to a large flower head. The
plant has large, broad lower leaves which are oval and arranged alternately on the stem and
smaller, narrower upper leaves which are attached individually to the stem. The flower head is a
large disc reaching 10–30 cm (4–12 in) in diameter which is made up of 16–30 individual florets
which are yellow-gold in color. The outer florets are sterile and produce the outer petals of the
flower head, while the inner florets will mature into the seeds in the central disc. Sunflowers are
annual plants, harvested after one growing season and can reach 1–3.5 m (3.3–11.5 ft.) in height.
Sunflower may also be referred to as girasol and originates from North America. it can be grown
in Northern Nigeria at Zaria, Gboko, and katsina Ala katsina state. (George et al,2018).

7
2.2.4 Uses

Sunflower seeds can be eaten either fresh or cooked or used to extract oil which is widely used in
cooking. The seeds are commonly harvested for bird seeds. Sunflowers are often grown as
ornamental plants due to their large, attractive flower head. (Ndoye, 2017).

2.2.5 Method of Propagation

i. Requirements 

Sunflowers are generally very easy to grow and thrive in areas with long hot summers which
promote flowering. They grow best at temperatures between 21 and 25.5°C (70–78°F).
Sunflowers can be very large and require plenty of space although there are some varieties which
have been specially bred to be compact for growing in smaller spaces or for growing in
containers. (Putnam et al, 2014).

ii. Planting

Sunflowers are most easily grown by direct seeding outdoors. In areas with a long growing
season, they should be planted in late Spring after all danger of frost and when the soil has
warmed through. However, in areas with short growing seasons, the seeds can be planted a week
or two before the last frost date as the plants are tolerant to cold Prepare the soil for planting by
digging to loosen the soil and break up any large clumps. Plant seeds 2.5–5.0 cm (1–2 in) deep
and space them 10–15 cm (3–4 in) apart. If planting in rows, allow 0.75 m (~30 in) between each
one. An application of a balanced fertilizer at planting promotes the development of a strong root
system. The seeds should sprout in 7–10 days. When the seedlings are about 15 cm (6 in) tall
with two pairs of true leaves, thin the plants to a final within row spacing of 60 cm (2 ft). Sow
more seeds every 2–3 weeks for a continuous bloom over the summer. (Myers et al, 2019).

iii. General care 

8
Although sunflowers are drought resistant, frequent, deep watering promotes the development of
a strong root system. The plants do not require fertilizing, indeed, addition of nitrogen promotes
vegetative growth and will delay flowering. The stems of the plants can easily reach in excess of
1.8 m (6 ft) in height and will benefit from some support. Bamboo stakes work
well. (Myers,2019).

Iv. Harvesting 

Sunflowers are ready to harvest when the back of the flowers begin to turn yellow and the flower
head droops. Cut the stem about 5 cm (2 in) below the head and hang up to dry in a warm, well
ventilated place for several weeks. When the heads are thoroughly dried, remove the seeds with a
brush or by hand. Allow the seeds to dry out for a further few days before storing. (Putnam et
al,2019).

2.3 AN OVERVIEW OF BIO LUBRICANT

2.3.1 Lubrication and Lubricant: Lubrication occurs when two surfaces are separated by a
lubricant film. A lubricant is a substance that reduces friction and wear by providing a protective
film between two moving surfaces. Lubricants are available in liquid, solid, and gaseous forms.
Bio lubricants are made from plants such as palm, soybean, sunflower, rapeseed, cassia tora seed
and coconut. Bio lubricants can also be made from synthetic esters and petroleum oil that satisfy
established biodegradability and toxicity criteria. Bio lubricants are generally considered as
lubricants with high biodegradability as well as low human and environmental toxicity.
Producing bio lubricants is suitable for alternative energy applications because of their
widespread sources. The types of bio lubricant feedstock may differ from country to country and
highly depend on geographical locations. Bio lubricants are made from different crop oils.More
than 350 oil-bearing crops are known, among which, only palm, soybean, sunflower, coconut,
safflower, rapeseed, cottonseed, and peanut oils are considered as potential alternative bio
lubricants. Palm oil is the main feedstock for bio lubricants and biodiesel in Malaysia. Moreover,
other non-edible oils such as jatropha, neem, and karanja have received worldwide interest.
(Jiang et al., 2018).

9
Biodegradability is the capability of a material to be decayed by microorganisms. A lubricant is
classified as biodegradable if its percentage of degradation in a standard test exceeds a certain
marked level. Vegetable oils exhibit better biodegradability than mineral oils and others. The
ecotoxic property of lubricating materials depends on the base oils and additives used in their
production. Biodegradability is primarily influenced by the base oil of lubricants. It depends on
the chemical structures of organic compounds. The chemical composition of base oils changes
during the application of lubricants, that is, when they are introduced to factors such as air,
temperature, metals, humidity, and pressure. The property changes of chemical structures during
service are responsible for biodegradability. ( Kombe et al,2018).

2.3.2 CHARACTERISTICS OF A GOOD LUBRICANT

A good lubricant exhibits the following characteristics:

i. High viscosity index (VI)

ii. high boiling point

iii. Thermal stability

iv. Low freezing point

v. Corrosion prevention capability, and

vi. High resistance to oxidation.

2.3.3 Purpose of Lubrication

The main purposes of lubrication are:

i. To reduce wear and heat loss that result from the contact of surfaces in motion, that is, to
reduce the coefficient of friction between two contacting surfaces;

ii. To prevent rust and reduce oxidation;

iii. To act as an insulator in transformer applications; and

iv. To act as a seal against dirt, dust, and water.

2.3.4 Applications of Bio lubricant
10
 i. Automotive oils: Oil Used in the automobile and transportation industry; examples are
engine oils, transmission fluids, gear box oils, as well as brake and hydraulic fluids.
ii. Industrial oils: Oil used for industrial purposes; examples are machine oils, compressor
oils, metal-working fluid, and hydraulic oils
iii. Special oils: Oil used for special purposes according to specific operations; examples are
process oils, white oils, and instrumental oils.

2.3.5 The Physiochemical Properties of Bio lubricants

Bio lubricants have many valuable and useful physicochemical properties. They offer technical
advantages unlike those of typical petroleum-based lubricants. Bio lubricants have high lubricity,
high VI, high flash point, and low evaporative losses. Overall, vegetable oil-based bio lubricants
exhibit several excellent properties compared with mineral oils. (Cai et al,2015).

Table 2.2 Shows the comparative analysis result of properties of vegetable oils.
Properties Vegetables oils Mineral oils
Density at 20®c(kg/m3) 940 880
Viscosity Index 100…200 100
Shear Stability Good Good
Pour Point (oc) ‒ 20…. + 10 ‒ 15
Clod flow behavior Poor Good
Miscibility with Good –
mineral oils Not miscible Not miscible
Solubility in water Moderate Good
Oxidation stability Poor Good
Hydrolytic stability Poor Good
Sludge forming Slight Sliyht
tendency
Seal swelling tendency

11
 Source: (Erhan et al, 2018)

i. Viscosity

Viscosity is the most important property of oil. It indicates resistance to flow, and is directly
related to temperature, pressure, and film formation. High viscosity indicates high resistance to
flow and low viscosity implies low resistance to flow.

ii. Viscosity Index (VI)

The VI indicates changes in viscosity with changes in temperature. A high VI indicates small
changes in temperature, whereas a low VI indicates high changes in temperature. Vegetable oil-
based bio lubricants have higher VI than mineral oils, which ensures that bio lubricants remain
effective even at high temperatures by maintaining the thickness of the oil film. Hence, bio
lubricants are suitable for a wide temperature range.

iii. Pour Point

Pour point is the lowest temperature at which oil flows or pours. Pour point is an important
factor. Vegetable oil-based bio lubricants have lower pour points than mineral oils, thus
providing excellent lubrication for cold starts.
iv. Flash Point and Fire Point

Flash point is the lowest temperature at which a lubricant must be heated before it vaporizes.
When mixed with air, a lubricant will ignite but will not burn. By contrast, fire point is the
temperature at which the combustion of a lubricant continues flash and fire points identify
lubricant volatility and fire-resistance properties. Both factors are important for transportation
and storage requirements. Vegetable oil-based bio lubricants have higher flashpoint than mineral
oils, thus considerably reducing the risks of fire in case of a lubricant leak, and providing safety
on shop floors.

(Honary et al., 2010).

v. Cloud Point

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Cloud point is the temperature at which solids dissolve in oil.Wax crystallizes and becomes
visible when temperature drops. To prevent clogging of filters, temperature must be maintained
above the cloud point.
vi. Acid or neutralization Number
The acid or neutralization number indicates the amount of acid or base content required by a
lubricant for neutralization.
vii. Oxidation Stability
Oxidation stability is the ability to exhibit resistance toward oxide-forming tendency, which
increases when temperature rises. The most significant contributors to oxidation include metal
surfaces, temperature, contaminants, pressure, agitation, and water. A low oxidative stability
indicates that oil oxidizes rapidly during use if it is untreated, becoming thick and polymerizing
to a plastic-like consistency.

viii. Rust and corrosion Prevention

Rust is chemical reaction between water and ferrous metals; meanwhile, corrosion is a chemical
reaction between chemicals and metals. Vegetable oil-based bio lubricants are nontoxic and react
less with chemicals, water, and ferrous metals than mineral oils.

ix. Anti-wear Properties

Lubricants are satisfactory for low-speed and low-pressure applications. Boundary lubrication
occurs when oil viscosity is insufficient to prevent surface contact. Anti-wear additives provide a
defensive film at contact surfaces to reduce wear. Anti-wear property is identified by standard
laboratory tests. Vegetable oil-based bio lubricants have better anti-wear properties than mineral
oils. ( Asadauskas S, et al., 1996).

2.3.6 Advantages and disadvantages of bio lubricants over conventional lubricant

Vegetable oils can be used as lubricants in their natural form. They have several advantages and
disadvantages when considered for industrial and machinery lubrication

13
(Conventional lubricant)

A. ADVANTAGES

vegetable oils have excellent lubricity, which is far superior compared with that of mineral oils.
Vegetable oils also have a high VI. For example, a VI of 223 is common among vegetable oils,
whereas a VI of 90–100 is normal for most mineral oils. Another important property of vegetable
oils is their high flash points. Typically, the flash point of vegetable oils is 326 1C, whereas that
of common mineral oils is 200 1C. More importantly, vegetable oils are biodegradable, generally
less toxic, renewable, and reduce dependency on imported petroleum oils.

Table 2.3 Some summarized benefits of bio lubricants over conventional

High lubricity Lower friction losses, better fuel economy
Low volatility Decreased exhaust emissions.
High viscosity index Used for wide temperature range.
High boiling temperatures Less emissions
High detergency Eliminating the requirement of detergent
additives
High flashpoints Higher safety on shop floor
Rapid biodegradation Reduced toxicological and environmental
hazards.
Oil mist and oil vapor reduction Leads to less breathing of oil mist inti the
lungs.
Better skin compatibility High cleanliness and less dermatological at
work place.

14
 A. DISADVANTAGES

vegetable oils in their natural form lack sufficient oxidative stability for lubricant application.
Low oxidative stability indicates that oil will oxidize rapidly during use if untreated, becoming
thick and polymerizing to a plastic-like consistency. Vegetable oils also have low-temperature
limitations, unpleasant smell, poor compatibility with paints and sealants, flushing propensity
because of low viscosity, and filter-clogging tendency. (Goyal et al., 2013).

Table2.4 Summary of the work done by various researchers on vegetable oil based bio-
lubricant.

Bio lubricants Reference lubricant Test methods and Result Reference

condition
Coconut oil SAE 20W50 Four-ball tester Less coefficient of friction, Higher (Jayadas
anti-wear property, Better et al, 2017)
lubricities properties

Waste palm oil l SAE 40 Four-ball tribo- (Kalam

tester, with, Lower coefficient of friction, et al, 2016)
Standard test Lower coefficient of friction
method lp-239. Higher viscosity
,
Vegetable oils Petroleum base oils Different tribo- High flash point, High viscosity (Singh
(Jatropha, tester with standard index, High lubricity, low et at, 2017)
Neem, Karanja, test method. evaporative loss, offer better
Soybean, Palm, Cassia performance, less expensive,
tora, mineral oil Cheaper and friendly.
Coconut, Castor, Olive,
Mahua, Sunflower, etc.)

Castor Oil Super refined mineral Four-ball tester Greater viscosity index, lower (Asadauskas
oil deposit forming tendencies, lower et al, 2016)
volatility, higher concentrations of
antioxidants.
Soybean Oil Petroleum based oil Four– ball wear Less coefficient of friction, beter (Adhvaryu
tester lubricity property. et at, 2019)
Palm oil base TMP SAE 40 High frequency Good wear prevention property, in (Erhan et al,
ester reciprocating terms of coefficient of friction. 2018)

15
 machine
Castor oil and palm oil SAE 20W40 Pin on dic tribo Excellent lubricity properties, (Zulkifli
water, tribo metre possess lower volatility. et al, 2018)
Pongamia oil SAE 20W40 Four skroke, single Lesser frictional losses, improve (Maleque
cylinder, water. the efficiency. et al, 2017)
Jatropha oil SAE 20W40 Pin on dic machine Lower wear loss & friction (Beka et al,
coefficient 2018)
Chemically modified SAE 20W40 High frequency Good oxidative stability, improve (Jaina et al,
repseed oil bio lubricant reciprocating cold flow property. 2017)
tribometre test rig
Soybean oil Commercial synthetic High frequency Extremely large viscosity. (Arumugam
lubricant reciprocatin et at, 2019)

16
2.7 Optimization of the oil Produced

Most optimization methods entail the application of statistical software to optimize the control
variables (extraction time, sample weight, solvent volume, nature of solvent, seeds’ variability,
and particle size, etc.) that seek reduce cost and increase performance while at the same time
minimizing deterioration of the quality of the product as much as possible. With respect to oil
extraction, two main methods of process optimization can be identified in the literature: the
traditional or conventional optimization method in which a single variable is changed at a time
instead of all simultaneously, sometimes referred to as single parameter optimization and that in
which a number of variables can be varied simultaneously to take care of interactions that can
occur between the factors known as design of experiments (DOE). (Ndoye,2007).

2.7.1 Importance of Optimization

Optimization speed application development, simultaneously empowers developers to create

more feature for further improving business and increasing profitability.

i. Increase productivity in process plant.

ii. Payback time is usually measured in mouths and sometimes in days.

iii. Optimization helps to generate the highest return on investment in industry.

iv. Optimization is synonymous with reducing cost.

2.8 Response surface methodology (RSM)

Response surface methodology (RSM) is a collection of mathematical and statistical techniques

in which a response of interest is influenced by several variables and the objective is to optimize
this response using any of the model of equation 2.1 or 2.2.

Y (%)= f (x1 + x2) + E. …………………………………….. ……………………..2.1

17
where y represents the noise or error observed in the response y and surface represented by ῃ = f
(x1, x2), which is called a response surface and

Y(%)=β0+β1x1+β2x2+β3x3+β1x12+β2x22+β3x32+β1x1x2+β2x1x3+β3x2x3+e….................... 2.2

where y is the predicted response factor, β0 is the intercept value, βi is the first order model
coefficient. And x1, x2j and x3 represents quadratic coefficients and e is the random error.The
main objective of RSM is to optimize the response which are usually represented graphically
called surface response, where ῃ is plotted versus the levels of x 1 and x2, to help visualize the
shape of a response. In the contour plot, lines of constant response are drawn in the x 1 & x2
planes, each contour corresponds to a particular height of the response surface.(George et al.,
2017).

2.9 Design of Experiments (DOE)

2.9.1 Box-Behnken Design

Box-Behnken proposed three level designs for fitting response surfaces. Each factor, or
independent variable. A Box-Behnken design is a three – level quadratic design that does not
contact fractional factorial design. The sample combination are treated in such a way that they
are located at midpoints of edges form by any two factors. The design is rotatable (or in cases,
nearly rotatable). (George Box 1960) advantage in statistics, Box-Behnken designs are
experimental designs for response surface methodology, devised by George E.P. Box and
Donald Behnken in 1960, to achieved the following goals, each factor, or independent variable,
is placed at one if the three equally spaced values, usually coded as -1,0, +1. (at least three levels
are needed for the following goals).The design should be sufficient to fit a quadratic model, that
is, one containing squared terms, product of two factors, linear terms and intercept. The ratio of
the number of the experimental points to the number of coefficients in the quadratic model
should be reasonable (in fact, designs kept in the range of 1.5 to 2.6).

The estimation variance should be more or less depend only on the distance from the center (this
is archive exactly for the designs with 4 and 7 factors). And should not vary too much inside the
smallest (hyper) cube containing the experimental points.

One advantage of Box-Behnken design is that it requires fewer design point than a full factorial
design CCD and additionally, a Box-Behnken Design avoid extremes, allowing you to work
18
around extreme factor combinations. Considered using the Box-Behnken design DOE type if
your project has parametric extremes (for example, has extreme parameter values in corner that
are difficult to build), since the Box-Behnken DOE doesn’t have corners and doesn’t combined
parametric extremes can reduce the risk of update failures. (Box-Behnken,2019).

2.9.2 Characterization of oil from both seeds (sunflower/cassia tors seeds)

This helps to identify the product in terms of it purity by carrying out some series of analysis.

2.9.3 Specific gravity

Specific gravity is the ratio of the density of a substance to the density of a reference substance
equivalent, it is the ratio of the mass of a substance to the mass of a reference for the same given
volume at a specific temperature that is 298k, which is always less than one (Roberts, 2006).

2.9.4 Refractive Index

Refractive index is the ratio of the velocity of light in vacuum to the velocity of light in a
medium.it is an indication of the level saturation of the oil.

2.9.5 Density

The density was determined by putting some quality of the sample oil in a beaker of known
mass. the final weight of the beaker is noted after the sample is poured into the beaker. The
volume of the oil is also noted after which the density is evaluated using the relationship density
is mass per unit volume g/cm3.

2.9.6 Yield

The extracted oil is transferred into a measuring cylinder. The measuring cylinder is then placed
over water bath for complete evaporation of solvents in a hot air oven as reported by Warra et al.
(2011).and volume of the oil was recorded and expressed as oil content (%)using the
mathematical relationship below:

Yield (%)=final weight of oil / initial weight of sample 100……….………………… 2.3

19
 CHAPTER THREE

3.0. MATERIALS AND METHOD

The various types of chemicals and equipment that were used to carried out the experimental
work for this research are listed as follows:

TABLE 3.1: List of Chemicals

S/NO Reagents Sources

1. Hydrochloric acid Chemical Eng’g Lab

2. Methanol Chemical Eng’g Lab

3. Ethanoic acid Chemical Eng’g Lab

4. Concentrated Sulphuric acid Chemical Eng’g Lab

20
 5. Potassium hydroxide Chemical Eng’g Lab

6. Ethelene glycol

7. Sodium methroxide

8. Phenolphthalein Chemical Eng’g Lab

9. Wiji’s solution Chemical Eng’g Lab

10. Distilled Water Chemical Eng’g Lab Chemical Eng’g Lab

11 Ethanol Chemical Eng’g Lab Chemical Eng’g Lab

12 Potassium iodide Chemical Eng’g Lab

Table 3.2 List of Apparatus and Equipment

S/N Equipment/Apparatus Manufacturers

1 Beaker Pyrex, England

2 Burette Pyrex, England

3 Ph meter Hannah inst. Corning-Ltd
USA
4 Pippete Pyrex, England
5 Thermometer Zeal England
6 Retord stand
7 Measuring cylinder Pyrex, England

21
 8 Weighing balnce Ohaus scale corp. Melrose Pack,Iinois
9 Stop Watch Smiths, Germany
10 Heating mantle Brain Weighs, England
11 Digital temperature sensor Zeal, England

3.2 Process Block Diagram

Sunflower and cassia tora oils

Blending of the oils

Characterization of the
blended oil

22
Esterification process
 1st Trans-esterification 1 blended oil
process
2 potassium hydroxide

2nd Trans-esterification 13 fame

methanol
process 2 Ethylene glycol
3 sodium methroxide

Biolubricant

Characterization of the bio

lubricant

3.3 Sample Collection and Preparation

The cassia tora oil was bought from Narrate analytical laboratory Zaria, while sunflower oil was
bought at central market Kaduna. Both oils were blended and characterized base on the
physiochemical properties:

S/NO: Variables Symbols -1 0 +1

1. Temperature (°C) A 48 54 60
2. Time (min) B 60 90 120
3 Amount of Catalyst (g) C 0.4 0.6 0.8
Table 3.4.1. Table of input variable values of experiment design and the code

23
Table3.4.2 Table of model matrix for experimental coded value

Std Run Oder Factor 1 Factor 2 B:Time Factor 3 Response Yield (%)

Order A:Temperature (oC) (min) C;Catatlyst (g)

2 1 60 60 0.6
8 2 60 90 0.8
7 3 48 90 0.8
6 4 60 90 0.4
10 5 54 120 0.4
1 6 48 60 0.6
3 7 48 120 0.6
9 8 54 60 0.4
15 9 54 90 0.6
12 10 54 120 0.8
11 11 54 60 0.8
5 12 48 90 0.4
4 13 60 120 0.6
14 14 54 90 0.6
13 15 54 90 0.6

3.4 Methodology for Bio lubricant Production.

3.4.1 Preparation of sunflower/cassia tora oils blending

The two different oils (sunflower and cassia tora oils) each 0.75litres were blended manually to
make up 1.5litres blend oil. The blending was done in order to improve on their physio chemical
properties of both the blended oil and the bio lubricant to be produced.

3.4.2 Procedure

3.4.2.1 Oil esterification for free fatty acid conversion

of Potassium hydroxide in order to determine the Free fatty acid (FFA) content of the sample In
order to curb the risk of exposing the oils to saponification, the free fatty acids (FFAs) in the oil

24
were reduced by reacting the oil with pure ethanol and ethanoic acid in the presence of sulphuric
acid as catalyst; 50ml of the blended oil was weighed and transferred into a separate beaker. 1ml
of pure ethanol and 1ml of ethanoic Acid were mixed in a test tube, 2 to 3 drop of concentrated
sulphuric acid (H2SO4) was also added and mixed up together. The content of the Test tube was
then poured in 50ml of the blended oil and stirred together to have a homogeneous mixture.
After twenty minutes of stirring, the sample was titrated against 0.1 molar solution.

The FFA value was then calculated using

Acid value = A × M × 56.1 /weight of sample(g)

Then ,free fatty acid = acid value/2

3.4.2.2 Transesterification

The process synthesis of the bio-lubricants involved a-two stage transesterification so as to

reduce the FFAs in the oil to appreciable limit; the first stage was aimed at producing an
intermediate product (methyl-ester / bio diesel/ Fame) from the blended oil, while the

second stage involved the conversion of the methyl-esters formed to produce the polyol esters of
the oil as shown below:

3.4.2.3 Methyl ester (biodiesel) synthesis

50ml of the blended oil sample was trans-esterified with methanol in the ratio of 10%w/w using
potassium hydroxide (KOH) as catalyst. the time of the experiment used was from 60, 90 and
120 (mins). while the amount of catalyst used are 0.4, 0.6 and 0.8(g) respectively, and a fixed
temperature of 48,54 and 60 (oC ) were used as shown in table 3.4.1, in order to account for the
yield of the methyl esters as intermediate product.

3.4.2.4 Polyol ester (bio-lubricant) synthesis

50ml methyl esters (FAME) obtained from the 1st stage of transesterification was reacted with
ethylene glycol in the ratio of 5%w/w in batches using sodium methoxide as the catalyst. this
was done so as to bring about the 2nd stage transesterification. Based on the results from RSM in

25
table 3.4.2, the amount of catalyst used were 0.4,0.6 and 0.8 (g). the total reaction temperatures
are 48, 54 and 60 °C.

CHAPTER FOUR

4.0 RESULT AND DISCUSSION

This chapter presents the results of bio lubricant production and the results of optimization of the
yield “viscosity index” using Box Behrkhen design with design expert software version 7.1.6 .

Table 4.1 Response Surface Methodology Experimental Runs and Results of Yield.

Std Run Oder Factor 1 Factor 2 Factor 3 Response 1 Viscosity Index

Order A:Temperature B:Time (min) C;Catatlyst (kg/m/s)

( C)
o
(g)
2 1 60 60 0.60 140

26
 8 2 60 90 0.80 137
7 3 48 90 0.80 162
6 4 60 90 0.40 131
10 5 54 120 0.40 144
1 6 48 60 0.60 180
3 7 48 120 0.60 151
9 8 54 60 0.40 149
15 9 54 90 0.60 138
12 10 54 120 0.80 142
11 11 54 60 0.80 150
5 12 48 90 0.40 168
4 13 60 120 0.60 134
14 14 54 90 0.60 138
13 15 54 90 0.60 138

Table 4.1 Shows the result obtained from the optimization of the biolubricant from
sunflower/cassia tora blended oil. The optimizing was carried out using response surface
methodology with Box Berhnken design (BBD), design – expert software version 7.1.6 was used
to optimized the effect of the three selected variables: time, temperature and amount of catalyst,
and the result shows that temperature and catalyst have a great effect on the optimization of the
biolubricant, the lower the temperature, the more the response yield. Likewise the higher the
catalyst the more the response yield.The overall analysis indicated that run (6) gave the highest
significant effect compared to the others. While the responses showed the viscosity index (180),
acid value (0.5386 mgKOH/g), FFA (0.2693), viscosity (69.16),, saponification value (127.347

mg/g), peroxide value (38.00 meq/kg) and iodine value (10.6596 mg/g )respectively. therefore, it
Indicates a significant effect for bio lubricant production.

Table 4.2: Analysis of variance Table for Anova

Source Sum of Squares df Mean Square F-value p-value

Prob< F

Model 2634.40 12 219.53 6.366E + 007 < 0.0001 Significant

A-temperature 961.00 1 961.00 6.366E + 007 < 0.0001 Significant

B-time 42.25 1 42.25 6.366E + 007 < 0.0001 Significant

27
 C-catayst 0.25 1 0.25 6.366E + 007 < 0.0001 Significant

AB 132.25 1 132.25 6.366E + 007 < 0.0001 Significant

AC 36.00 1 36.00 6.366E + 007 < 0.0001 Significant

BC 2.25 1 2.25 6.366E + 007 < 0.0001 Significant

A² 251.31 1 251.31 6.366E + 007 < 0.0001 Significant

B² 92.31 1 92.31 6.366E + 007 < 0.0001 Significant

C² 39.00 1 39.00 6.366E + 007 < 0.0001 Significant

ABC 0.000 0

A²B 60.50 1 60.50 6.366E + 007 < 0.0001 Significant

A²C 0.13 1 0.13 6.366E + 007 < 0.0001 Significant

AB² 3.13 1 3.13 6.366E + 007 < 0.0001 Significant

AC² 0.000 0

B²C 0.000 0

BC² 0.000 0

A3 0.000 0

B3 0.000 0

C3 0.000 0

Pure Error 0.000 2 0.000

Cor Total 2634.40 14

Table 4.2 shows analysis of variance table ( partial sum of squares - type III ) anova for
response surface cubic model (Aliased). Statistical analysis of the model was performed to
evaluate the anova and check the adequacy of the empirical model. The results of anova for
fitting the quadratic response surface model by a mean square method are summarized in
table 4.5. The coefficients of the response surface model in actual factor were also evaluated.
The significance of each of the coefficients are checked from p-values, which also indicate the
interaction strength of each parameter.
The model f-value of 63660000.00 implies the model is significant. There is only a 0.01%
chance that a "model f-value" this large could occur due to noise. Values of P - Value, "prob > f"
28
less than 0.0500 indicate model terms are significant. In this case A, B, C, AB, AC, BC, A 2, B2,

C2, A2B, A2C, AB2 are significant model terms. Values greater than 0.1000 indicate the model
terms are not significant. If there are many insignificant model terms (notcounting those required
to support hierarchy), model reduction may improve the model.

Table 4.3: Model coefficient for response surface in terms of coded factors
Factor Coefficient df Standard 95% CI 95% CI VIF
Estimate Error Low High

Intercept 138.50 1

A-temperature - 15.50 1 2.00

B-time - 3.25 1 2.00

C-catayst - 0.25 1 2.00

AB 5.75 1 1.00

AC 3.00 1 1.00

BC - 0.75 1 1.00

A² 8.25 1 1.01

B² 5.00 1 1.01

C² 3.25 1 1.01

ABC ALIASED Intercept

A 2B - 5.50 1 2.00

A²C 0.25 1 2.00

AB² 1.25 1 2.00

AC² ALIASED A,AB²

B²C ALIASED C,A²C

BC² ALIASED B,A²B

A³ ALIASED A

B³ ALIASED B

29
C³ ALIASED C

Table 4.3: Shows model coefficient for response surface cubic model in terms of coded Factors.
The model coefficients and probability values i.e coded values shown in Table 4.6. the low
values of the standard error obsessed in the intercept and all the model terms showed that
regression model fits the data well and the prediction is good. The variance inflation Factor VIF
obtained in this work showed that the center points are orthogonal to all other factor in the
model. The model also proved suitable for the adequate representation of the real relationship
among the selected independent, the coefficient estimate represents the expected change in
response per unit change in factor value when all remaining factors are held contact. The
intercept in orthogonal design is the overall average response of all the runs. The coefficients are
adjusted around that the average based on the factor setting. When the factor are orthogonal the
VIFs are 1, VIFs greater than 1 indicate multi co - linearity, the higher the VIF the more the
severe the correction of factors. As a rough rule, VIFs less than 10 are tolerable.

4.1 Model Summary Statistics

Source Std Dev R- Squared Adj R-Squared Pred R- Square PRESS
Linear 7.24 0.7813 0.7217 0.6193 1003.03 Suggested
2F 7.2 0.8460 0.7305 0.5484 1189.75
Quadratic 3.57 0.9758 0.9322 0.6128 1020.00 Suggested
Cubic 0.00 1.0000 1.0000 Aliased
Table 4.4 Analysis of variance ( ANOVA) of the regression equation.
Std. Deviation 3.57 R-Squared 0.9758

Mean - Adj R-Squared 0.9322

C.V. % Pred R-Squared 0.6128

PRESS 1020.00 Adeq Precision -

Table 4.4 Shows the value of regression coefficient of determination (R2) for the model was
0.9758 and adjusted (R2) is 0.9322 both indicating the good fitness of the model. With this, it

30
indicates an adequate signal from the result that the model can be used to navigate the design
space.
4.2 Determination of Optimum Yield.
Final equation in terms of actual factors.
The experimental analysis of table 4.1 was used to obtained the second order statistical model
coefficients of equation 4.1. the empirical model equation for the biolubricant yield were
developed using experimental datas in table 4.1, and are described as equation 4.1 below,as
function of the reaction temperature, time and amount of catalyst.

Viscosity index (yield) ¿ 138.00 – 15.50 (Temperature) −¿ 3.25 (Time) −¿ 0.25 (Catayst) +
5.75 (Temperature × Time) + 3.00 (Temperature × catalyst) −¿ 075 (Time × Catalyst) + 8.25
(Temperature) 2
+ 5.00 (Time) 2 + 3.35 (Catalyst) 2
– 5.50 (Temperature) 2
× (Time) + 0.25
(Temerature) 2 × (Catalyst) + 1.25 (Temperature) × (Time) 2 ……………………………4.1

Substituting for the optimum values,the yield can be calculated from equation 4.1.

Viscosity index (Yield)= 138.00 – 15.50 (48) −¿ 3.25 (60) −¿ 0.25 (0.6) + 5.75 (48 × 60) +
3.00 (48 × 0.6) −¿ 075 (60 × 0.6) + 8.25 (48) 2 + 5.00 (60) 2 + 3.35 (0.6) 2 – 5.50 (48) 2 × (60) +
0.25 (48) 2 × (0.6) + 1.25 (48) (60) 2 = 86.462%

The result of the optimization for biolubricant production wsa presented in Table 4.1. the yield of
each run of the experiment was determined using Equation 4.1. the optimum biolubricant yield
of 180, reaction Temperatuer 48 oC,60 minute reaction Time, and 0.6 amount catalyst. While the
calculated optimum yield is 86.462%.
Table 4.5 Comparison physiochemical properties of cassia tora bio lubricant, sunflower bio
lubricant, blended cassia tora & sunflower bio lubricant and conventional lubricant.
Parameters Cassia tora Sunflower Blended Conventional
biolubricant lubricant

31
Yield (%) 52.74 56.48 68.21 ---
Density (kg/m )3
0.8891 0.905 1.2783 0.860
Viscosity at 40oC 47.52 45.24 69.16 45
Viscosity at 100 C o
28.93 23.11 44.17 6.5
Specific gravity 0.9981 1.471 1.2789 0.8979
Viscosity index 169 158 180 140
Saponification value 79.1 ± 197.4 127.347 ---
Acid value 1.80 0.19 0.5386 0.8962
Free fatty acid 0.945 0.095 0.2693 ≤ 0.4621
Peroxide value 48.2 56.12 38.00 ---
Iodine value 100 124 10.6596 ---
Cetene number ---- ---- 87.6174 ---

Table 4.5 Shows the comparison of physiochemical properties of cassia tora bio lubricant,
sunflower bio lubricant, blended cassia tora & sunflower bio lubricant and conventional
lubricant. the physio chemical properties of biolubricant produced was compered with that of the
conventional lubricant, from the above comparison, base on the overall analysis on the
physiochemical properties, the result shows that, the biolubricant produced gave the highest
significant effect when compared to that of conventional. It has high viscosity index of 180,The
VI indicates changes in viscosity with changes in temperature. A high VI indicates small changes
in temperature, whereas a low VI indicates high changes in temperature. Vegetable oil-based bio
lubricants have higher VI than mineral oils, which ensures that bio lubricants remain effective
even at high temperatures by maintaining the thickness of the oil film. Hence, bio lubricants are
suitable for a wide temperature range.It also have a viscosity of 69.16 and 44.14 at 40 oC and at
100 oC respectively whit low acid and FFA values. This Viscosity is the most important property
of oil. It indicates resistance to flow, and is directly related to temperature, pressure, and film
formation. High viscosity indicates high resistance to flow and low viscosity implies low
resistance to flow. So from the above parameters shows a greater significant effect when
compared to the conventional lubricant.

32
Table 4.6 Comparison of physiochemical properties of crude cassia tora oil, crude
sunflower oil and blended cassia tora/sunflower oil.

Parameters Crude cassia tora Crude sunflower Blended oil

oil oil
Yield (%) 57.76 41.3 59.38
Density (kg/m )3
0.890 0.878 0.837
Viscosity at 40 oC 51.22 48.32 53.83
Viscosity at 100 C o
38.90 26.60 42.36
Viscosity Index 103.74 14.45 123.1
Specific gravity 0.88 0.9162 0.86
Acid value 1.46 0.953 4.18
Free fatty acid 0.73 0.4765 2.09
Peroxide value 40 28.322 52.0
Iodine value 8.12 9.6 10.0152

Table 4.6 Shows the comparison of physiochemical properties of crude cassia tora oil, crude
sunflower oil and blended cassia tora/sunflower oil. The physio chemical properties were
determined according to ASTM standard, the blending was done in other to see if there is going
to an improvement or changes in the physio chemical properties of the oil, also to check if the
blending will fit be used for the biolubricant production. From the result gotten shows almost
all the parameters are fit for the production except the acid value and Free fatty acid are found
to be high which indicates that the FFA must have to reduced to a minimal value less than 1 for
it to fit for the production, before the production, the FFAs were reduced to a minimal levels as
shown in Appendix A.

4.2 Effect of Process variable on biolubricant yield using the Optimized yield model.

33
The response surface plot shown in figure 4.1 to 4.3 shows the optimal condition between
independent variables in different fixed parameters.
Design-Expert® Software
120.00
viscosity
viscosity
Design Points
180

131 105.00

B : tim e
X1 = A: temperature
X2 = B: time

Actual Factor 90.00 151.053

C: catalyst = 0.80

158.54 143.566

75.00
166.026

173.513

60.00
48.00 51.00 54.00 57.00 60.00

A: temperature

Design-Expert® Software

viscosity
Design points above predicted value
Design points below predicted value
180

131
v is c o s it y

X1 = A: temperature 180
X2 = B: time
166.25
Actual Factor 152.5
C: catalyst = 0.60
138.75

125

120.00 60.00

105.00 57.00

90.00 54.00

75.00 51.00
B: time A: temperature
60.00 48.00

Figure 4.1 Response surface ploting using 3D surface and contour plot of viscosity, time and
temperaturet.

34
 Design-Expert® Software
0.80
viscosity
viscosity
Design Points
180

131 0.70

136.382

C : c a ta ly s t
X1 = A: temperature
X2 = C: catalyst

Actual Factor 0.60 155.353149.029 142.705 3

B: time = 90.00

0.50
161.676

0.40
48.00 51.00 54.00 57.00 60.00

A: temperature

Design-Expert® Software

viscosity
180

131

X1 = B: time
v i s c o s it y

X2 = C: catalyst
151
Actual Factor
A: temperature = 54.81 147.75

144.5

141.25

138

0.80 120.00

0.70 105.00

0.60 90.00

0.50 75.00
C: catalyst B: time
0.40 60.00

Figure 4.2 Response surface ploting using 3D surface and contour plot of viscosity, catalyst and
time.

35
 Design-Expert® Software

viscosity
180

131

X1 = C: catalyst
X2 = A: temperature

v is c o s it y
163
Actual Factor
B: time = 87.57 155.25

147.5

139.75

132

60.00 0.80

57.00 0.70

54.00 0.60

51.00 0.50
A: temperature C: catalyst
48.00 0.40

Design-Expert® Software
60.00
viscosity
viscosity
Design Points
180
A : te m p e r a tu r e

131 57.00

X1 = C: catalyst
X2 = A: temperature 136.382

Actual Factor 54.00 3

B: time = 90.00
142.705

51.00 149.029

155.353

161.676
48.00
0.40 0.50 0.60 0.70 0.80

C: catalyst

Figure 4.3 Response surface ploting using 3D surface and contour plot of viscosity, temperature
and catalyst.
Figure 4.1 Shows the response surface ploting using 3D surface and contour plot for viscosity,
time and temperaturet and result shows that viscosity is decreasing with decrease in time,and
decreasing with increase in temperature. figure 4.2 shows the response surface ploting using 3D
surface and contour plot of viscosity, catalyst and time. The result shows the viscosity is
decreasing with decrease in both catalyst decreasing with increase in time. Figure 4.3 Shows the
response surface ploting using 3D surface and contour plot of viscosity, temperature and catalyst.
The result shows that at viscosity is increasing with increase in both temperature and catalyst.

36
 Design-Expert® Software
viscosity
Normal Plot of Residuals
Color points by value of
viscosity : 99
180
95
131
90

80
70

50

30
20

10
5

-1.26 -0.43 0.40 1.23 2.06

X: Internally Studentized Residuals

Y: Normal % Probability

Figure 4.4 Response graph of predicted Vs actual.

Predicted vs Actual values plot for response in Figure 4.4. shows the closeness of the
experimente values donate by the dotted point to the predicted. This shows that the pridicted
model with coefficient of R² = 0.9758 %, can be used to predict the biolubricant yield of the
experimental observe values. The Figure 4.4 shows that values obtained follow the predicted
values indicating that the model assumptions fit the statistics.

37
 CHAPTER FIVE

CONCLUTION AND RECOMMEENDATION

5.1 CONCLUSION

Base on the findings the following conclusions are made

 The blend of sunflower cassis tora oil was successfully characterized having a density of
(0.837), Specific gravity (0.86) viscosity (53.83), (viscosity index (123.1), acid value of
(4.18mgKOH/g). FFA (2.09),peroxide value (52.00meq/kg), and iodine value
(10.0152mg/g) respectively.
 Biolubricant from the blends of sunflower and cassia tora oil was produced through Box
Behrkhan design with design expert software.The best output response was achieved at the
reaction temperature of 48 oC, 60 minutes reaction time, and 0.6 amount of catalyst.
 The properties of biolubricant produced was compared with that of conventional lubricant
which has viscosity of 69.16,viscosity index 180,FFA 0.2693,acid value 0.5386 while that of
conventional has viscosity of 45,viscosity index 140,FFA 0.4621, and acid value 0.8962
respectively.

5.2 RECOMMENDATION

1) Further systematic research should be conducted to confirm the tribological behavior of

different biolubricant from different blended oils.
2) Further research work should be conducted using different approach of design model to
ascertain the most preferred optimization model on the blended oil from different seeds.

38
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41
 APENDIX A

Calculation for Acid Value and Free Fatty Acid

A × 56.1
Acid value =
Weig h t of sample( g)

acid value
Free fatty acid =
2

Run 1

0.6 ×0.1 ×56.1

AV = = 0.6732mgKOH/g
5

0.6732
FFA = = 0.3366mgKOH/g
2

2. AV = 0.4488mgKOH/g

FFA = 0.2244mgKOH/g

3. AV = 0.8976mgKOH/g

FFA = 0.4488mgKOH/g

4. AV = 0.561mgKOH/g

FFA = 0.2805mgKOH/g

5. AV = 0.7854mgKOH/g

FFA = 0.3927mgKOH/g

6. AV = 1.0098mgKOH/g
42
 FFA = 0.5049mgKOH/g

7. AV = 0.9761mgKOH/g

FFA = 0.4881mgKOH/g

8. AV = 1.0210mgKOH/g

FFA = 0.5105mgKOH/g

9. AV = 0.6059mgKOH/g

FFA = 0.3029mgKOH/g

10. AV = 0.6732mgKOH/g

FFA = 0.3366mgKOH/g

11. AV = 0.5386mgKOH/g

12. AV = 0.6732mgKOH/g

FFA = 0.3366mgKOH/g

13. AV = 0.7181mgKOH/g

FFA = 0.3590mgKOH/g

14. AV = 0.6283mgKOH/g

FFA = 0.3142mgKOH/g

15 AV = 0.7405mgKOH/g

FFA = 0.3703mgKOH/g

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 APPENDIX B

Calculation for Peroxide value

( S ‒ B ) × No of t h iosulfate × 1000
PV =
Weigh t of sample (g)

Run 1

( 10.5 ‒ 8.9 ) ×0.1 ×1000

PV = = 38mg/g
5

2. PV = 20.8mg/g

3. PV = 32.6mg/g

4. PV = 48.6mg/g

5. PV = 44.8mg/g

6. PV = 18.00mg/g

7. PV = 22.2mg/g

8. PV = 30.8mg/g

9. PV = 38.00mg/g

10. PV = 53.00Mmg/g
44
11. PV = 38.00mg/g

12. PV = 34.00mg/g

13. PV = 42.4mg/g

14. PV = 43.6mg/g

15. PV =44.00m/g

APPENDIX C

Calculation for Iodine Value

( S ‒ B ) × N × 12.69
Iodine value =
Weig h t of t h e sample

Run 1

( 49 ‒ 44.99 ) × 0.1× 12.69

IV = = 10.2789mgI/100kg
0.5

2. IV = 11.4464mgI/100kg

3. IV = 10.6342mgI/100kg

4. IV = 10.6849mgI/100kg

5. IV = 10.8118mgI/100kg

6. IV = 13.1215mgI/100kg

7. IV = 10.4058mgI/100kg

8. IV = 11.1672mgI/100kg

9. IV = 17.0299mgI/100kg
45
10. IV = 15.4057mgI/100kg

11. IV = 10.6596mgI/100kg

12. IV = 12.5123mgI/100kg

13. IV = 12.9438mgI/100kg

14. IV = 17.8168mgI/100kg

15 IV = 15.9894mgI/100kg

APPENDIX D

Calculation for Cetene Number

5458
CN = 46.3 + – (0.225 × 10)
SV

Run 1

5458
CN = 46.3 + ‒ 0.225 × 10.2787 = 79.6902
128.8725

2. CN = 86.2559

3. CN = 82.2484

4. CN = 88.8857

5. CN = 96.4568

6. CN = 76.7521

7. CN = 99.0067

8. CN = 78.5761

46
9. CN = 79.9059

10. CN = 80.2532

11. CN = 87.6174

12. CN = 93.0910

13. CN = 92.4032

14. CN = 94.1795

15 CN = 74.9796

APPENDEX E

Calculation for Viscosity

The viscosity is calculated using digital viscosity meter at 40% and 100%

Run 1 Viscosity at 40 oC = 65.52, at 100 oC = 40.47

Run 2 Viscosity at 40 oC = 55.22, at 100 oC = 42.2

Run 3 Viscosity at 40 oC = 78.23, at 100 oC = 46.74

Run 4 Viscosity at 40 oC = 74.97, at 100 oC = 44.97

Run 5 Viscosity at 40 oC = 59.43, at 100 oC = 35.02

Run 6 Viscosity at 40 oC = 60.17, at 100 oC = 41.18

Run 7 Viscosity at 40 oC = 65.52, at 100 oC = 43.47

Run 8 Viscosity at 40 oC = 65.52, at 100 oC = 41.03

47
Run 9 Viscosity at 40 oC = 69.18, at 100 oC = 39.97

Run 10 Viscosity at 40 oC = 50.88, at 100 oC = 36.88

Run 11 Viscosity at 40 oC = 69.16, at 100 oC = 44.17

Run 12 Viscosity at 40 oC = 81.16, at 100 oC = 42.47

Run 13 Viscosity at 40 oC = 63.97, at 100 oC = 35.17

Run 14 Viscosity at 40 oC = 65.32, at 100 oC = 46.21

Run 15 Viscosity at 40 oC = 8, at 100 oC = 31.51

APPENDIX F

CALCULATION FOR VISCOSITY INDEX

the Viscosity index of the bio lubricant were calculated and determined using ISO Viscosity machine

Run 1 VI = 138

Run 2 VI = 137

Run 3 VI = 162

Run 4 VI = 151

Run 5 VI = 140

Run 6 VI = 142

Run 7 VI = 138

48
Run 8 VI = 138

Run 9 VI = 150

Run 10 VI = 131

Run 11 VI = 180

Run 12 VI = 134

Run 13 VI = 144

Run 14 VI = 149

Run 15 VI = 180

49