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CHARACTERIZATION AND MODIFICATION OF CASTOR OIL EXTRACTED

FROM THE NEWLY MALAYSIAN PRODUCED CASTOR BEANS

WAN ALIUDDIN BIN WAN RAZDI

Thesis submitted in fulfillment of the requirements

For the award of the degree of
Bachelor in Chemical Engineering

Faculty of Chemical Engineering and Natural Resources

UNIVERSITY MALAYSIA PAHANG

JANUARY 2012
 v

ABSTRACT

Vegetable oils, either edible or non-edible, are widely used in huge number of
applications in industry. Ricinus communis (castor plant) is one of the non-edible
vegetable oil and its usage in many industries as a raw material and additives is rapidly
growing. In this research, the Malaysian newly produces castor beans are extracted and
the castor oil is characterized. The castor oil that is obtained from extraction is refined
and modified for further uses. The extraction process involve four steps which are
clearing, drying, winnowing and also grinding to get high yield of oil. The castor cake
then extracted using the soxhlet extractor and hexane as the solvent. The extracted
castor oil produced is characterize by determining the acid value, saponification value,
iodine value, specific gravity, viscosity of the oil, the refractive index, and pH value.
The crude oil from the extraction process then refines by degumming and neutralization
process and then the neutralize oil is bleached. The Malaysian castor oil properties are
compared with the ASTM standard specifications. The conclusion is the properties of
Malaysian crude and refined castor oil is determined and be compared with the world
standard specification of castor oil. The refined castor oil then modified for further uses.
The different castor seed from different area which is Casa 5 and Casa 101 is extracted
to obtain the castor oil and identify which location in Malaysia that the castor seed
produces more oil content and have the same standard with world castor oil quality.
 vi

ABSTRAK

Minyak sayuran, samada boleh dimakan atau tidak boleh dimakan telah banyak
digunakan dalam pelbagai kegunaan di dalam industri. Pokok castor adalah sejenis
minyak sayuran yang tidak boleh dimakan dan banyak digunakan di dalam pelbagai
industri sebagai bahan mentah dan bahan tambahan. Dari penyelidikan ini, biji castor
yang baru dihasilkan di Malaysia diekstrak dan di sifatnya fizikal dan kimia nya di kaji.
Proses mengekstrak minyak castor di mulakan dengan membersihkan, mengeringkan,
mengupas dan menghancurkan biji castor untuk memperoleh peratusan minyak yang
tinggi. Biji castor yang hancur diekstrak menggunakan pengekstrak 'Soxhlet' dan hexane
sebagai pelarut. Minyak castor yang di peroleh dari biji castor yang diekstrak di tapis
dan di ubahsuai untuk kegunaan lain. Minyak castor yang diperoleh di kaji kualitinya
dari segi nilai asid, nilai iodin, nilai kelikatan, nilai index biasan, nilai pH, nilai
SG(specific gravity) dan nilai SV(saponification value). Minyak mentah kemudiannya
di tapis dengan proses penyah-gam(degumming), di neutralkan dan dilunturkan. Sifat
minyak castor di bandingkan dengan ASTM kualiti. Kesimpulannya, minyak mentah
dan minyak ditapis dan ditulenkan di banding sifatnya dengan kualiti minyak castor
antarabangsa. Minyak yang ditapis di ubahsuai untuk kegunaan lain. Biji castor yang
ditanam di kawasan yang berbeza diekstrak dan mengenalpasti kawasan mana di
Malaysia yang menghasilkan biji castor yang dapat mengeluarkan banyak minyak dan
mempunyai kualiti minyak setaraf dengan kualiti minyak castor dunia.
 1

CHAPTER 1

INTRODUCTION

1.1 RESEARCH BACKGROUND

The Vegetable fats or vegetable oils have an essential function in the

industrial economy of a developing country as the seed oil provide a huge use in
human daily life in order to complete and make the nowadays life more easier. The
seed oils are one of the vegetable oil family members. Vegetable oils or vegetable
fats are the lipid materials that been derived from the natural plants which physically
oil are in liquid state in the room temperature whereas the fat exists in solid state in
the room temperature (Ndiaye et. al., 2006). The vegetable oil is composed of
triglycerides which lack glycerin in its structure.

Oils that are extracted from plants have been used in this world since the
ancient times and already used in many cultures. As an example the castor plant has
been known to man for ages. Castor beans have been found in ancient Egyptian
tombs dating back to 4000 B.C and during that time, the castor oil was used
thousands of years ago in the wick lamps for lighting (Scarpa et. al., 1982).
Basically, to obtain the oil from the plants or seeds, the seeds and the plants are
through extraction process and then be distillate to remove the solvent used as to
separate the extracted oil and solvent used in order to get the pure oil (Kirk-Othmer,
1979).

Several feedstocks from vegetable source such as soybean, rape seed, canola,
palm, corn, Japtropha and castor seeds have been studied as an alternative to oil
candidate. Among these sources, castor seeds are a potentially promising feedstock
since among vegetable oils, castor oil is distinguished by its high content (over 85%)
 2

of ricinoleic acid. There is no other vegetable oil contains so high a proportion of

fatty hydroxyacids and castor oil is the most stable viscosity of any vegetable oil
(Ogunniyi, 2006).

There are variety processes or the combination of the processes to obtain the
oils from the castor seeds. The hydrate presses, continuous screw presses and also
solvent extraction are the common methods to obtain the oils from the castor seeds.
However, the most satisfactory approach to get the oil is hot pressing the castor
seeds by using a hydraulic press and then followed by solvent extraction. This
proposal is however focused at extraction of castor oils using solvent. The castor
seed firstly face the separation process of the shell from the nibs and then by using
the mortar and pestle, the seeds were crushed into the paste (cake) to release the
castor fat for the extraction process (Ogunniyi, 2006).

1.2 IDENTIFICATION OF PROBLEM

Currently, the leading producers and the countries that seriously involve in
the production of castor oils are India, China, and Brazil. Together, these countries
account for 90% of the acreage and production of castor beans. It is grown in Costa
Rica, Ecuador, Thailand, Philippines, Paraguay, Romania, Sudan, Mexico, Pakistan,
Ethiopia, and Tanzania. The world-wide production stood at 1, 227, 669 tonnes in
2000 (FAO). However, India is the world’s largest producer of castor seeds and oils
that meets most of global demand for castor oil. India contributes about 750, 000
tonnes annually, and accounting for 60% of the entire global production. Essentially,
all the castor oil production in the U.S has been eliminated by a combination of
economic factors, excessive allergenic reactions of field and the processing workers,
and the toxicity of the seed meal. The toxic inside the castor seed which is known as
ricin, is a very dangerous to human as it can kill adults if two or three castor seeds
were chewed (Ogunniyi, 2006).

In Malaysia, the castor seeds have been planted in order to fulfill the demand
for castor seeds. Casa Kinabalu Sdn.Bhd. is the company that is responsible in the
production and the planting the castor plant in Malaysia. This company still new in
Malaysia and the first castor seeds that harvest in Malaysia was at the end of
 3

October 2010. Casa Kinabalu Sdn.Bhd already plant the castor beans about 7000
acres in Lundu, Sarawak, 30 acres in Gua Musang, 10 acres in Lukut, Negeri
Sembilan, 5 acres in Muar, 10 acres in Kulai, Johor, and also 20 acres in Kedah.
Unfortunately, all the castor beans that obtain are exported to the China. Based on
the situation happen, we are proposing to extract the newly Malaysian castor seeds
in order to obtain the oil that the oils than be characterize and compare the physical
and chemical properties of Malaysian castor oil with global castor oil properties. The
castor oil extracted than will react with sulphuric acid in process called sulphation to
modify the refined castor oil (Ogunniyi, 2006) .

1.3 STATEMENT OF OBJECTIVES

The main objectives of this study are to extract the castor oil by using the
different extraction method, characterize the crude and refined castor oil that then be
modified using sulfation method for newly Malaysian castor bean.

1.4 RESEARCH SCOPES

The research scopes for this study are:

i. To extract the castor oil from Malaysian castor seed by using soxhlet
extractor and solid-liquid extraction to compare the product percentage oil.
ii. To characterize the crude and the refined castor oil for easy identification
and also assess it quality by combining the extracted oil quality with the
national castor oil standard.
iii. To determine either the Soxhlet extraction process or Solid-Liquid extraction
can give more percentage of oil
iv. To extract the crushed castor seed(kernel together with husk) and compared
the oil obtained with dehuled castor seed(kernel only)
v. To modified the refined castor oil for another uses.
 4

1.5 RATIONALE AND SIGNIFICANCES OF STUDY

Due to the importance of the vegetable oils in the industrial, pharmaceutical,

food industries, and also medical, there is an urgent need to produce more oil from
the natural plant. In view of this, castor oil is a promising vegetable oil because it
has several advantages; it is renewable, environmental friendly and produce easily in
the rural areas, where there is an acute need for modern forms of energy. The
primary use of the castor oils is as the basic ingredient in the production of nylon 11,
sebacic acid, plasticizers and engine jet lubricant. Castor oil’s high lubricity which
reduces the friction is superior to other vegetable oils and petroleum-based
lubricants. It is really clings to metal, especially hot metal, and the castor oils is used
in production nylon 6-10, heavy duty automotive greases, coating and inks,
surfactants, polyurethanes, soaps, polishes, synthetic resins, fibers, paints, varnishes,
dyes, leather treatments, hydraulic fluids and also sealants(Ogunniyi, 2006).
Specification for pharmaceutical use can be found in the European Pharmocoepia.
The industrial type maybe divided into three types of quality. ‘First’ quality is the oil
that obtains from only one pressed castor oil and extracted without solvent. This
kind of oil normally produced in Europe, is virtually colorless and has very low
acidity. ‘Second’ and ‘third’ quality of castor oil is commercial names, meaning that
the oil has been extracted using solvent (Ogunniyi, 2006).

The oils from the castor seed are very well known as a laxative and purgative
that has been widely used for over 2, 000 years. This oil is so effective that it is
regularly used to clear the digestive tract in cases of poisoning. The castor oil also
has a remarkable antidandruff effect. It is well tolerated by the skin and so is
sometimes used as a vehicle for medicinal and cosmetic preparations. When the
alcoholic solution is distilled in the presence of sodium salts of higher fatty acids,
castor oil congeals to a gel-mass. This useful gel is used in the treatment of
dermatosis and is good protective in cases of occupational eczemas and dermatitis.
Medical applications consume a tiny fraction of total production. The castor seeds
and residual cake are highly poisonous and unless processed to remove the poisons
cannot be fed to livestock (Anandan et. al., 2005). In some countries, castor cake is
 5

used as a fertilizer. The poisons or the toxics that contain in the castor cake include
ricin (Burdock et. al., 2006).
 6

CHAPTER 2

LITERATURE REVIEW

2.1 BASIC FACTS ABOUT CASTOR OIL

The trade in castor oil as an item of commerce goes back to antiquity

(Ogunniyi, 2006). The castor oil is obtained from the extracting method or pressing
the castor seed which known with botanical name Ricinus Communis. This oil is
inexpensive, environmentally friendly and also a naturally-occurring resource. The
oil that comes from castor is a viscous, pale yellow color, non-volatile, and also non-
drying oil with a bland taste and sometimes used as a purgative. Furthermore, the oil
has a slight characteristic odour while the crude oil tastes slightly acrid with a
nauseating after-taste. The oil is one of the relative in the vegetable oil family which
has a good shelf life and it does not turn rancid unless the oil subjected to excessive
heat. The largest exporter of castor oil is India and the other major producers of
castor oil are China and Brazil as shown Table 2.1. The total world production of the
extracted castor oil is about 500, 000 tonnes and the production of seeds are
estimated at one million tonnes (Ogunniyi, 2006).

Table 2.1: Production volume of Castor Oil by major producers

Source: Ogunniyi, (2006)

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2.1.1 The Castor Oil Properties

Relative to other vegetable oils, castor oil has different physical and
chemical properties which vary with the method of extraction the oil. The castor oil
that obtain from the cold pressing has low acid value with low iodine value and has
slightly higher saponification value compared to the solvent-extracted oil, and the oil
is lighter in color (Ogunniyi, 2006). The typical properties are shown in the table 2.2
and the representative composition of oil is given in figure 2.1. The chemistry of
castor oil is focused on its high content of ricinoleic acid and also the other three
points of function that exist in the castor molecule. One of the molecule functions is
the carboxyl group that can give a huge and wide range of the esterifications. Second
one is the single points of unsaturation which can be altered using the hydrogenation
process or the epoxidation process or the vulcanization process. The last one is the
hydroxyl group in the castor oil can be acetylated or alkoxylated maybe can be
remove from the oil molecule by using the dehydration process to increase the
unsaturation of the oil compound to provide the semi-drying castor oil. By high-
temperature pyrolysis and by caustic fusion, the hydroxyl position of oil which is so
reactive the molecule can be split at that point to yield useful product with shorter
chain length. Actually, the presence of the hydroxyl group on the castor oil is adding
the extra stability to the castor oil and also preventing the formation of
hydroperoxides.

Table 2.2: Characteristics of castor oil in different situation

Source: Ogunniyi, (2006)

 8

Figure 2.1: Equation showing the constitution of castor oil (Ogunniyi, 2006)

The ricinoleic acid that exists inside the castor oil comprises over 89% of the
fatty acid of the oil. The other fatty acids that present are linoleic acid (4.2%), oleic
acid (3.0%), stearic acid (1%), palmitic acid (1%), dihydroxystearic acid (0.7%),
linolenic acid (0.3%), and eicosanoic acid (0.3%) (G. R. O’Shea Company).

Figure 2.2: Composition of castor oil fatty acids

 9

The castor oil consists mainly of ester of 12-hydroxy-9-octadecenoic acid

(ricinoleic acid) as the present of hydroxyl groups and the double bonds makes the
oil suitable for many chemical reaction and modification. Various reaction of castor
oil is given in table 2.3. Furthermore, the oil is characterized by high viscosity
although this is unusual for a natural vegetable oil (Turner et. al., 2004). This
behavior is due largely to hydrogen bonding of its hydroxyl groups. The castor oil is
soluble in the alcohols in any proportion. However, this oil is limited solubility in
aliphatic petroleum solvents. Castor oil is a unique naturally-occurring polyhydroxy
compound that has the limitation which is the hydroxyl value and acid value is
reducing on the storage. The acid value and hydroxyl value may change about 10%
if the oil is stored for about 90 days. The reason why this situation happened is the
reaction between the hydroxyl and carboxyl group of oil molecule to form estolides.

Table 2.3: Production a variety of derivatives from chemical reaction

Source: Ogunniyi, (2006)

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2.2 FEATURES OF CASTOR SEEDS

The castor plant grows in the wild in large quantities in most tropical and
sub-tropical countries. The plant is available at the low price and it is known to
tolerate in varying weather condition. Normally, the castor plant needs a temperature
between 20 and 26 °C with low humidity throughout the growing season in order to
give maximum yield. Moreover, the weather conditions for its growth limit its
cultivation to tropical areas of the developing world. There are different types of
castor seeds all around the world but on the average, the castor seeds contain about
30 to 55% of oil by weight. The seeds are very poisonous to human and also animals
as the seeds contain ricin, ricinine and certain allergens which are toxics. The effects
if the castor seed is accidentally ingested, the victims will face abdominal pain,
vomiting and diarrhea and as little as 1 mg of the ricin can bring the human to death.
The fear of accidental ingestion of the poisonous castor seed by the children does
not encourage the use of the castor plant for ornamental purpose. Besides that, the
seed cake is poisonous and consequently not suitable for animal feed. Some people
who worked with the meal highly develop allergic reaction such as asthma. The
main reason why the US farmers no longer grow the castor plant is because of the
toxicity of castor seed extensively. However, the pure castor oil if used in right and
recommended quantities can be used as the laxative. The quality of the seed oil is
hardly affected by the variation in good or poor seeds. The oil from the castor seed is
non-edible oil which can be used and can free up some edible oils used in industries
for human consumption. The castor plant and castor seed are shown in figure 2.3
and figure 2.4.
 11

Figure 2.3: The castor plant

Figure 2.4: The castor seed

Source: Ogunniyi, (2006)

 12

2.2.1 Extraction of Castor Seed Oil

There are many ways to obtain the oil from the castor seeds. The extraction
of oil from the castor seed is one or combination of processes, such as mechanical
pressing and solvent extraction. The examples of the mechanical pressing are
hydrate presses and continuous screw presses. However, the most effective way to
obtain the oil from the seed is hot pressing using a hydraulic press and followed by
solvent extraction (Akpan et. al., 2004). In the mechanical pressing, the seeds are
crushed to remove the seed from the shell and the adjusted to low the moisture
content by warming in a steam-jacketed vessel or in the oven. After that, the crushed
seeds are placed into the hydraulic presses and the seeds are pressed by until become
the cake to extract the oil. The properties of oil from the mechanical pressing are the
oil has the light colour and low free fatty acids (Ogunniyi, 2006). However, about
45% of oil present by the mechanical pressing and the remaining oil in the castor
cake can be recovered only by the solvent extraction method. During extraction
method using solvents such as heptanes, hexane and petroleum ethers, the seed
cakes are extracted with the solvent in the Soxhlet extractor or the commercial
extractor.

2.2.2 Refining the Castor Oil

As in other vegetable oils, it is a usual process to refine the crude oil that
obtained from either mechanical pressing or solvent extraction. The main objective
of refining is to remove the impurities like colloidal matter, free fatty acid, colouring
matter and other undesirable constituents, thus making the oil more resistant to
deterioration during storage. Refining process includes several steps. Firstly, the
solid and colloidal matters are removed by settling and filtration. Then, free fatty
acid of the oil is neutralizing by using the alkali. The coloured matter is removes by
bleaching process and lastly, the oil will face the deodorizing step by using the
treatment with steam at high temperature and low pressure. The standard method of
refining the edible oil is applicable to the castor oil.
 13

2.3 USES OF CASTOR OIL

Although the castor oil is not edible oil, it is more versatile than other
vegetable oils as the castor oil is widely used as a starting material for many
industrial chemical products because of its unique structure. The castor oil is one of
those vegetable oils that have found usage in many chemical industries. It is the raw
material for many chemical products and also as the additives in drugs. The usage of
castor oil can be divided into industrial, food, medicine and also biodiesel and
biofuel industries.

2.3.1 Industrial castor oil

As the castor oil is non-edible oil, it is very useful to replace the edible that
used in industries. The castor oil has numerous uses in transportation, cosmetics and
pharmaceutical and manufacturing industries. For example, the castor oil is used as
the adhesives(Yeadon et. al., 1959), brake and hydraulic fluids (Shough, 1942),
caulks, dyes, electrical liquid dielectrics, lubricating greases, machining oils,
paints(Nezihe, et. al., 2011), pigments, polyurethane adhesives(Kirk-Othmer, 1979),
refrigeration lubricant, washing powder, sealants, textiles, waxes, leather treatment,
and lacquers. The vegetable oils are very interesting due to their good lubricity and
biodegradability as they are attractive alternatives for petroleum-derived lubricants,
but the vegetable oils has the weakness as oxidative stability and low temperature
performance limits their widespread uses. Not like the other natural vegetable oils,
the castor oil has better low temperature viscosity properties and also high
temperature lubrication than most of vegetable oils. So, the castor oil is very useful
as the lubricant in jet, diesel and race car engines. Castor oil also used in the
industries as the raw material for the production of a number of chemicals such as
notably sebacic acid which is used in plasticizer and manufacture of dioctyl sebacate
(a jet lubricant), undecylenic acid (perfume formulation) (Das et. al., 1989) and also
nylon-11.
 14

2.3.2 Castor oil in food

Castor oil is used in the food industry as the food additives, flavourings,
candy like chocolate, as a mold inhibitor and also in packaging. The castor oil is
known as the non-edible oil which means the castor oil is not save to eat. By using
the cold press process, the castor oil that obtain is safe to eat as the cold press oil
contain low acidic and iodine value (Burdock et. al., 2006). The polyoxyethylated
castor oil is also used in the foodstuff industries.

2.3.3 Medicinal use of castor oil

The castor oil is categorized as ‘generally recognized as safe as effective’

(GRASE) by the United States Food and Drug Administration (FDA), for over the
counter use as a laxative, with its major site of action the small intestine. However,
although it may be used for constipation, it is not a preferred treatment. Undecylenic
acid, a castor oil derivative, is also FDA approved for over the counter use on skin
disorders or skin problems. Nowadays, the modern drugs are rarely given in a pure
chemical state, so, the most active content of the medicine combined with the
additives. The castor oil or the castor oil derivative is added to many modern drugs.
The examples are Miconazole (an anti-fungal agent), Paclitaxel (a mitotic inhibitor
used in cancer chemotherapy), Nelfinavir mesylate (an HIV protease inhibitor),
Xenaderm ointment (a topical treatment for skin ulcers), and Aci-jel (used to
maintain the acidity of the vagina).

2.3.4 Castor oil as Biodiesel and Biofuel

The extracted castor oil which is called the crude castor oil, is refined and the
biofuel and biodiesel is produced through the process of esterification and
transesterification (Canoira et. al., 2010). The transesterification process is hugely
eliminates the tendency of the castor oils and fats to undergo the polymerization and
auto-oxidation process. This process also reduces the viscosity of the castor oil so
that the castor oil viscosity about the same as the petroleum diesel viscosity (Valente
et. al., 2011).
 15

2.3.5 Castor Meal

The castor meal or the castor cake waste is the excellent bio-fertilizer as it
contains optimal composition of nutrients especially N-P-K. The toxic called ricin in
the castor meal makes the castor meal unsuitable for animal feed. This situation
makes the price for castor meal is lower compared to the prices of soy meal and
rapeseed meal as both type of the meal can be used as animal feed. The high
fertilizer value in the castor meal with the lower price in the market makes the
demand for the castor meal increase from the organic fertilizer market.
 16

CHAPTER 3

RESEARCH METHODOLOGY

3.1 MATERIAL AND SOLVENT

Hexane (C6H14) is the solvent that will be used to extract the castor oil. The
mixture of diethyl ether (C2H5)2O and ethanol (C2H5OH) and few drop of
phenolphthalein with the titration process using 0.1M NaOH is used to determine
the acid value of oil. After that, 0.1N ethanolic potassium hydroxide with few drop
of phenolphthalein will be used to obtain the saponification value of the oil. The
carbon tetra chloride (CCl4) will be added with Wijs solution and aqueous potassium
iodide (KI) and then be titrating with 0.1M sodium-thiosulphate solution (Na2S2O3)
to determine the iodine value of the oil. The starch indicator is added when the
process to determine the iodide value of the oil. HCl is used to active the clay in the
refining process of extracted castor oil. NaOH and the sodium chloride are added in
the neutralization process of the extracted oil. Concentrated sulphuric acid (H2SO4)
is used in the modification process of the oil that obtains from the extraction process
and then be neutralizing using sodium hydroxide (NaOH).

3.2 APPARATUS

The apparatus that will be used in this experiment are oven, soxhlet extractor
and viscometer. Detail explanations are provided in Section 3.2.1, 3.2.2, and 3.2.3.
 17

3.2.1 Oven

Oven as illustrated in Figure 3.1 is the equipment that will be used in this
research for drying purposes. The oven is designed with maximum temperature of
220°C. The front panel located at the top of the unit provides a digital display of the
temperature reading in Centigrade. It has three levels of tray and drying process can
be set up by wall heat of by blowing hot air from the fan on the wall at the inside
back of the oven. Time consumption of drying process can be set up on lower part
of front panel so that the oven will be automatically reduce its temperature to
ambient temperature after drying process end.

Figure 3.1: Laboratory oven

 18

3.2.2 Soxhlet extractor

The soxhlet extraction is normally used when the desired product or

compound has a limited solubility in a solvent, and the impurity is insoluble in that
solvent. The simple filtration can be used to separate the compound from the
insoluble substance if the desired compound has a significant solubility in a solvent.
The material that containing some of the desired product will be placed inside the
thimble that made from the thick filter paper which is placed into the main chamber
of the soxhlet extractor. Then, the soxhlet extractor is placed onto a flask which
containing the extraction solvent and equipped with a condenser. During the
extraction process, the flask that contains the solvent is heated to reflux. The solvent
will vaporize up to distillation arm, and then flood into the chamber housing the
thimble of the material. The used of condenser is to make sure that the solvent vapor
that already cools drips back down into the chamber housing the material. The
chamber slowly fills with warm condensate solvent. Some of the desired compounds
will the dissolve in the solvent. As the extractor is almost full, the chamber will
automatically emptied by a siphon side arm, with the solvent running back down to
the distillation flask and the cycle will be allowed to repeat many times.

Figure 3.2: Laboratory soxhlet extractor

 19

3.2.3 Viscometer

Viscometer which is also known as viscosimeter is one type of laboratory

equipment which is used to measure the viscosity of a fluid. An instrument called a
rheometer is used to measure the liquid with the viscosities that vary with flow
condition. The viscometer is used to measure only one flow condition. In general,
either the fluid remains stationary and an object moves through it, or the object is
stationary and the fluid moves past it. The drag caused by relative motion of the
fluid and a surface is a measure of the viscosity. The flow conditions must have a
sufficiently small value of Reynolds number for there to be laminar flow.

Figure 3.3: Laboratory viscometer

3.3 EXPERIMENTAL WORK

The experimental work is shown in the figure 3.4. The experiment start with
the determination of oil content and then the oil is characterize. After that, the
extracted oil is refined and then be characterize again. Lastly, the refined oil is
modified using sulfation method.
 20

EXTRACTION

SOLID-LIQUID SOXHLET

OIL

CRUDE PREPARATION OF CLAY

CHARACTERIZATION DEGUMMING AND

NEUTRALIZATION

ACID VALUE

BLEACHING
SAPONIFICATION VALUE

IODINE VALUE REFINED

SPECIFIC GRAVITY

MODIFICATION
REFRACTIVE INDEX

VISCOSITY

pH VALUE

Figure 3.4: Flow of the experimental work

 21

3.3.1 Castor Beans Processing

The castor beans must undergo some step of processing before the extraction
procedure. Firstly, the castor seeds are cleaned as the seeds which are obtain from
hand picking, had some foreign material and dirt. The cleaned castor seeds then
placed in open area for sun dried until the casing splits and sheds the seeds. After
sun dried, the beans then go for further dried as the beans are place inside the oven
at 60°C for 7 hour to reduce its moisture content which normally castor bean contain
about 5 to 7% of moisture. After that, the shell is separated from the nibs (cotyledon)
by using the tray that blows away the cover in order to achieve high yield. By using
the mortar and pestle, the castor beans are crush into a paste which is called ‘cake’ to
weaken the cell wall to release castor fat during the extraction.

Clearing

Drying

Winnowing

Grinding

Figure 3.5: Flow chart of castor bean processing

3.3.2 Operation of Soxhlet Extractor

10g of the castor bean cake is placed in the thimble and inserted in the center
of the soxhlet extractor. 300ml of normal hexane is poured into a round bottom
flask. The soxhlet then heated at 60°C and as the solvent is boiling, the vapor rises
until the condenser at the top of the extractor. The condensate solvent then drip into
 22

the filter paper thimble in the center of the thimble which contain the castor cake to
be extracted. The extracted product then seeps through the thimble’s pores and flow
back down into the round bottom flask. The extraction is proceeding until 30
minutes. After that, the castor cake is remove from the tube and dried in the oven
and be cooled inside the desiccators. The castor cake is weighted again to determine
the amount of the oil that already extracted. The further extraction is proceeding at
30 minutes interval until the cake weighed at further extraction and the previous
extraction is same. The extraction then carried out for 5g of the castor cake. The
weight of the oil extracted is determined at 30 minutes time interval. The final step
to obtain the extracted castor oil is the mixture of the solvent and the extracted oil is
heated to recover the solvent from the oil.

The castor cake is placed in the extractor

The soxhlet is heated and the solvent vapour rises

The condensate solvent drip into cake

The castor oil drip into the solvent

The mixture of oil and solvent is heated to recover the solvent

Figure 3.6: Flow chart of operation of soxhlet extractor

3.3.3 Determination of Moisture Content of the Seeds

The cleaned castor seeds are weighed and then dried inside an oven that
operates at 80°C for 7 hours and the weight of the seed is take after at every 2 hours.
The step is repeated until the weight of the seed is constant. During the 2 hours
interval, the seeds are removed from the oven and the cooled inside the desiccators
for 30 minutes. The cooled seeds then remove from the desiccators and re-weighed.
The percentage of the moisture inside the castor seeds is calculated using the
 23

formula: Moisture= 100(W1-W2) / W2 %, where W1 = original weight of the castor

seed before drying and W2 = weight of the sample after drying.

The cleaned castor seeds are weighed and then dried inside an oven for 7 hours

The weight of the seed is take after at every 2 hours

The step is repeated until the weight of the seed is constant

Each two hours, the seed removed from oven and cooled before weight

The percentage of the moisture inside the castor seeds is calculated

Figure 3.7: Flow chart of determining the moisture content

3.3.4 Determination of the Percentage of Castor Oil Extracted

30g of castor seed that already crushed into the castor cake is place inside the
thimble and 300ml of the hexane as poured into the round bottom flask. The soxhlet
is heated at 60°C and the extraction is allowed for 3 hours continuously extraction.
The procedure is repeated by using the different weights of the castor cake. The final
step is the solvent which is the hexane, is removed by distillation process and the
percentage of extracted oil is determined.