Sesame Oil Extraction by Hexain
Sesame Oil Extraction by Hexain
Sesame Oil Extraction by Hexain
By Yared Abate
Adviser
Dr. Ing Berhanu Asefa
Assefa
June5, 2018
Declaration
Thesis is prepared by me. The thesis is entitled “Extraction and optimization of oil from sesame
seed by n hexane solvent”, It is submitted in partial fulfilment of the requirement for the Degree of
Masters Science in Addis Ababa Institute of Technology School of chemical engineering complies
with the regulation of the university and meets the accepted standards with respect to originality
and quality. I declare that it is done by myself and that it is not copied from other work.
i
Acknowledgments
Praise to God the Most Merciful and Compassionate for giving me the strength in completing
this research and thesis.
First and foremost, I would like to express my appreciation to my advisor, Dr-ing Berhanu Assefa
from Addis Ababa University, Addis Ababa Institute Technology (AAIT), Department of
Chemical Engineering for supervision, advice, guidance and patience throughout my research.
I also would like to convey my gratitude to a great number of laboratory assistant in AAIT
Chemical Engineering Department who’s helping me throughout the work especially Mr. Hintsa-
Selassie Seifu, Mr Nebiyu, Mr. Fasiel,
Finally, I would also like to thanks to Addis Ababa University for providing financial support for
this master’s thesis work.
At last, my appreciation is to my family especially my mother and sister. This thesis could not have
been completed without their patience and support.
Thank you.
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Table of Contents
..............................................................................................................................................................
Acknowledgments ................................................................................................................................ii
List of Tables ....................................................................................................................................... v
List of figures ...................................................................................................................................... vi
List of acronyms ................................................................................................................................ vii
Abstract ............................................................................................................................................viii
Chapter one .......................................................................................................................................... 1
Introduction ......................................................................................................................................... 1
1.1 Background .................................................................................................................................... 1
1.2 Problem of statement .................................................................................................................. 2
1.3 Objective ................................................................................................................................... 2
1.3.1 General Objective ................................................................................................................ 2
1.3.2 Specific Objective ................................................................................................................ 2
1.4 Significance ................................................................................................................................ 3
1.5 Scope of the Study ...................................................................................................................... 3
Chapter Two ........................................................................................................................................ 4
Review of Literature ............................................................................................................................ 4
2.1 Sesame seed history .................................................................................................................... 4
2.2 Production of sesame seed .......................................................................................................... 4
2.3 Sesame seed cultivation .............................................................................................................. 5
2.4 Sesame seed description ............................................................................................................. 7
2.5 Sesame oil description .............................................................................................................. 11
2.6 Extraction technology ............................................................................................................... 13
2.6.1 n-Hexane solvet extracion ...................................................................................................... 13
2.6.2 Supper critical extraction ................................................................................................... 15
2.6.3 Mechanical press extraction ............................................................................................... 17
2.7 Factors that Affect solvent extraction process ........................................................................... 18
2.7.1 Solvent Type...................................................................................................................... 18
2.7.2 Extractor Temperature ....................................................................................................... 19
2.7.3 Extraction Time ................................................................................................................. 20
2.7.4 Flakes Size (particle size)................................................................................................... 20
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2.8 Oil refinery ............................................................................................................................... 21
2.8.1 Degumming: chemical and physical refining...................................................................... 21
2.8.2 Neutralization: chemical refining ....................................................................................... 21
2.8.3 Bleaching: chemical and physical refining ......................................................................... 22
2.8.4 Winterization ..................................................................................................................... 22
2.9 Minor Components of Sesame Oil ............................................................................................ 23
2.10 Benefits of sesame seed processing ......................................................................................... 24
2.11 Use of byproduct .................................................................................................................... 25
Chapter Three .................................................................................................................................... 26
Material and Methods......................................................................................................................... 26
3.1 Materials needed to experiments ............................................................................................... 26
3.2 Methodology to this study ........................................................................................................ 27
3.2.1 Soxhlet extraction .............................................................................................................. 28
3.3 Characterization of sesame oil .................................................................................................. 31
3.3.1 Iodine value determination ................................................................................................. 31
3.3.2 Acid value determination ................................................................................................... 31
3.3.3 Gas Chromatography mass spectroscopy (GC/MS) result analysis ..................................... 32
3.3.4 Density measurement ......................................................................................................... 33
3.4 study design.............................................................................................................................. 33
3.5 statistical analysis and optimization .......................................................................................... 33
Chapter four ....................................................................................................................................... 35
Result and discussion ......................................................................................................................... 35
4.1 soxhlate extraction yield data .................................................................................................... 35
4.1.1 Effect of temperature on oil yield ...................................................................................... 38
4.1.2 Effects of Extraction Time on oil yield............................................................................... 39
4.1.3 Effects of moisture content on oil yield .............................................................................. 40
Chapter 5 ........................................................................................................................................... 46
Conclusion and Recommendation .................................................................................................. 46
5.1 Conclusion ............................................................................................................................... 46
5.2 Recommendation ...................................................................................................................... 46
References ......................................................................................................................................... 47
Appendix ........................................................................................................................................... 49
iv
Appendix A Integration Peak Area from Gas chromatography spectrometer ................................... 49
List of Tables
Table 2.1 Products of sesame and its uses ............................................................................................. 9
Table 2.2 Nutrient composition of sesame seeds Source (Williams, 2005) .......................................... 10
Table 2.3 Amino acid and fatty acid composition in sesame seeds Source (Williams, 2005) ............... 12
Table 3.1 Integration Peak List ........................................................................................................... 32
Table 3.2 soxhlate extraction Factors and their levels for central composite design ............................ 33
Table 4.1 The central composite design matrix and responses
Table 4.2 ANOVA for Response Surface Reduced Quadratic Model
v
List of figures
Figure 2.1 A Picture of the Sesame Plant with the Seed
…………………………………………………5
vi
List of acronyms
GCMS Gas chromatography mass spectroscopy
DT desolventizer Toaster
FFA Free fatty Acid
ALA alpha linolenic acid
RDA recommended daily allowance
KEYWORDS: Sesame seed, extraction, response surface methodology, oil yield, Design Expert.
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Abstract
Optimization of sesame oil extraction using response surface methodology (RSM) was carried out in
this study. The effects of three factors (moisture content of seed, extraction temperature and extraction
time) on the oil yield obtained from the seed were considered. With the aid of Design Expert and
using the central composite design of the response surface methodology, twenty (20) experiments
were generated and run. Using n-hexane as the solvent, each experimental run was carried out in
100ml Soxhlet extraction apparatus. The results obtained from the experiments together with the
factors considered during the experiments were modelled and analyzed using a quadratic model
based on observations made during the model analysis. The reults obtained from the quadratic model
for this extraction were R-squared, the adjusted R-squared and the predicted R-squared values of the
developed and modified quadratic model were 0.9986, 0.9975 and 0.9955. Also, with the aid of the
Design Expert, the optimum parameters of the process were estimated to be moisture content of 6%,
extraction temperature of 83 oC and extraction time of 7 hr. It was finally concluded that the optimum
values of the parameters given by the software were genuine ones, because the validation of the
optimum values obtained experimentally showed a very good conformity between the predicted
optimum oil yield and the experimental one. The quadratic models developed predicted 55.8% as
the maximum oil yield while the one obtained from the experiment was found to be 50.17%.
Therefore, the application of response surface methodology to optimize oil extraction from sesame
seed has been successfully demonstrated.
viii
ix
Chapter one
Introduction
1.1 Background
Sesame (Sesamum indicum) from Pedaliaceae, is an important oil seed crop being cultivated in the
tropics and the temperate zone of the world (Biabani and Pakniyat, 2008). It is one of the oldest oil crops
and is widely cultivated in Asia and Africa (Ali et al., 2007). It was a highly prized oil crop of Babylon
and Assyria at least 4000 years ago (Ross, 2005). This plant is called “sesame” internationally, while it
is called “benniseed” in West Africa, “simsim” in East Africa and“Till” in India. Within Ethiopia, it is
called “selit”. This crop is grown mostly for the oil extracted from its seed which is edible and use for
industrial and pharmaceutical purposes (Ogbonna and Ukaan2013). It ranks ninth among the top thirteen
oilseed crops which make up 90% of the world production of edible oil (Adeola et al., 2010).
Natural sesame oil derived from good quality seed has a very pleasant flavour and can be consumed
without further purification. The natural sesame oil has excellent stability due to the presence of high
level of natural antioxidants (Lyon, 1972).The oil is also useful in the industrial preparation of
perfumery, cosmetics (skin conditioning agents and moisturizers, hair preparations, bath oils, hand
products and make-up), pharmaceuticals, insecticides and paints and varnishes (Warra, 2011).
Generally, oil is extracted from sesame seed using methods like Soxhlet extraction, supercritical
extraction, etc. Soxhlet method is one of the most popular methods used for lipid extraction from natural
products and foodstuffs. According to this method, lipids are extracted from solids by multiple rinsing
out with an organic solvent like hexane or any low-boiling petroleum ether (Carvalho et al., 2012).
However, the efficiency of Soxhlet extraction, usually evaluated using oil yield has been discovered to
be affected by operating conditions such as temperature of extraction, seed size and extraction time. So,
in order to obtain good yield of oil from this seed, there is the need to obtain the optimum values of
these parameters affecting the extraction of oil from the seed.
1
1.2 Problem of statement
Edible oil is mainly produced from cotton seed, rape seed, lint seed, nigger seed, sesame seed, palm and
vegetables. In Ethiopia, the first two types are dominant in the market followed by lint and nigger seed.
Vegetable and palm oil are imported products while sesame oil is not easily available in the market.
Sesame is one of the major export earning oil seeds. Due to the highest price offer in the international
market as against the depressed price of domestic edible oil, the manufacturing of edible oil is mainly
processed from cotton seed and rape seed, which have lesser prices against sesame and other oil seeds.
Edible oil is part of everyday food expenditure in urban areas as well as in most of the rural areas.
Sesame oil is also used as an input for industrial production of pharmaceuticals, soap and cosmetics.
1.3 Objective
1.3.1 General Objective
Extraction of sesame oil from sesame seed using hexane solvent and optimization using surface response
method.
1.3.2 Specific Objective
To investigate the effect of moisture on the extraction process.
To investigate the effect of temperature on the extraction process.
To Optimize of Soxhlet extractor for different temperature, seed moisture content and extraction
time by using hexane solvent.
To Characterization of final oil at optimum condition such as acid value, FFA, iodine value,
density.
2
1.4 Significance
When this thesis project scale up to industry can create a job for many people. The establishment of such
factory will have a foreign exchange saving effect to the country by substituting the current imports. The
project will also create forward and backward linkage with the manufacturing sector and also generates
income for the Government in terms of tax revenue and payroll tax.
• This work will show the possibility of getting the oil and this can be used us an additive in soap and
cosmetic industries to improve the performance quality of the product.
• The experimental work showed that the possibility of getting the appropriate operating
conditions for extraction of sesame oil.
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Chapter Two
Review of Literature
2.1 History of sesame seed
Sesame seeds are the seeds of the tropical annual Sesamum indicum. The species has a long history of
cultivation, mostly for its yield of oil. The oil plant has been grown since the beginning of arable
cultivation, and originates from the dry bush savannah of tropical Africa, and spread from there to India
and China, where it is still widely cultivated. (Naturland, 2002).The original area of domestication of
sesame is obscure but it seems likely to have first been brought into cultivation in Asia or India
(www.nigeriamarkets.org). Archeological records indicate that it has been known and used in India for
more than 5,000 years and is recorded as a crop in Babylon and Assyria some 4,000 years ago (Borchani
et al., 2010).
Sesame was cultivated during the Indus valley civilization and was the main oil crop. It was probably
exported to Mesopotamia around 2500 BCE and was known in Akkadian and Sumerian as 'ellu'. Prior to
600 BC, the Assyrians used sesame oil as a food, salve, and medication, primarily by the rich, as the
difficulty of obtaining it made it expensive. Hindus used it in votive lamps and considered the oil sacred.
The largest producers are China and India, each with an annual harvest around 750,000 tonnes followed
by Myanmar (425,000 tonnes) and Sudan (300,000 tonnes). These figures are only rough estimates of
the situation as sesame is a smallholder crop and much of the harvest is consumed locally, without
record of the internal trade and domestic processing (CBN, 2009).
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2.3 Sesame seed cultivation
Sesame (Sesamum indicum L.) is a self-pollinating annual plant having a straight, pubertal stem with
branching and is known one of the most important oilseed crop. Sesame is a blossoming plant and
belongs to the genus Sesamum. Various wild relatives found in Africa and a minor number in India and
other parts of the world. It is extensively naturalize in tropical areas in the world. It is grown for their
edible seed that grows in pods. Its flowers are light yellow, although flowers are also differ in color with
various being purple or blue (Morris, 2002).
Sesame cultivation can be carried out on a wide range of soils but optimum are well-drained, loose,
fertile and sandy alluvial soils that have a pH value between 5.4 and 6.75. Very low pH values have a
drastic effect on growth, whereas some varieties can tolerate a pH value up to 8 (Naturland, 2002). Good
drainage is crucial, as sesame is very susceptible to short periods of waterlogging. Sesame is intolerant
of very acidic or saline soils (Bennet, 2011). The total amount of water required to grow sesame crop
ranges from 600 to 1000 mm, depending on the cultivar and the climatic conditions (Hansen, 2011).
Good harvests can be expected when rainfall of 300-600 mm is optimally spread throughout the
vegetation period. During each of its development stages, the plant is highly susceptible to water-
logging, and can therefore only thrive during moderate rainfall, or when irrigation is carefully controlled
in drier regions (Naturland, 2002). The water requirement can be met from available soil moisture at
sowing, rainfall during the growing season and irrigation (Hansen, 2011). This is because due to its tap
roots, the plant is highly resistant to drought, and can provide good harvests even when only stored soil
water is available. When irrigated, or during summer rain spells, sesame grows better in sandy than in
heavy soils. This is due to its sensitivity to high soil moisture contents (Naturland, 2002).
Sesame needs long periods of sunshine, and is generally a short-day plant, where by varieties exist
which are unaffected by the length of the day (Naturland, 2002). Sesame needs a constant high
temperature, the optimum range or growth, blossoms and fruit ripeness is 26-30°C. The minimum
temperature for germination is around 12°C, yet even temperatures below 18°C can have a negative
effect during germination (Naturland, 2002). Pollination and the formation of capsules is inhibited
during heat-wave periods above 40°C. In regions visited by strong, hot winds, the plants only form
smaller seeds with a lower oil content. Sesame is sensitive to strong winds when the main stem is fully
grown. Tall varieties should not be planted in regions which have strong winds during the harvesting
season (and, if necessary, hedges to protect against the wind should be planted) (Naturland, 2002). The
5
response of sesame to both temperature and daylength indicates that it should be cultivated in the wet
season in the tropics, or in the summer in the warmer temperate areas. While there is some variation
between cultivars, the base temperature for germination is about 16oC (Bennet, 2011). This warm-
season annual crop is primarily adapted to areas with long growing seasons and well-drained soils
(Hansen, 2011, www.nutrition-and-you).
Sesame is growing to 50 to 100cm (1.6 to 3.3ft) tall in length and it is an annual plant with conflicting
leaves 3 to 14cm (1.5 to 5.6 inch) extended with an whole edge; leaves are broad lanceolate, to 5cm (2
inch) wide at the bottom of the plant, lessening to just 1cm (0.4 inch) broad to the blossoming stem. The
floras are purple to white, cylindrical, 2 to 5cm (1.1 to 1.9 inch) long, lobed mouth with a four edges.
The seed cake is an excellent source of protein supplement in the animal feed industry. Sesame seed are
pear-shaped, ovate, small (about 2.5-3mm in length, 1.5mm in width), slightly flattened and thinner at
the helium. Weight of 1000 seeds is approximately 3g. Light-colored seeds yield better quality oil than
dark color but lower oil content (Mukhopadhyay and Ray, 1999).
6
2.4 Sesame seed description
Sesame has been considered crop that can be used as animal feed and human foods as a whole seed, oil,
and meal (Hahma et al., 2009). The sesame is not an excellent source of starch. The sesame seeds
contain approximately a quarter of soluble fibers out of the total fiber present in sesame. The main part
of soluble fiber is mucilaginous gum and its composition ranges from 8-11g per 100 g. The alpha
linolenic acid (ALA) which is an omega-3 fatty acid forms the major part of polyunsaturated fatty acids
in sesame. It is present about 50% of the total fatty acids. ALA is essential amino acid and cannot be
synthesized by the human body from any other substance therefore it is considered as an essential fatty
acid. The essential fatty acids requirements for the human body can be fulfilled by intake of sesame
products (Morris, 2004). A hundred grams of sesame provides 100% of the recommended daily
allowance (RDA) for manganese and potassium, 57-65% of the RDA of phosphorus and iron, and 13-
35% for zinc, calcium and copper while its recommended daily intake is 25 to 50 grams (Anon, 2006).
Specialty grains (bulgar wheat, barley, sesame, sprouted grains and rice extract) are used in breakfast
cereals to add novel textures, flavors and colors in these products.
The unique flavor and its opposition to oxidative corrosion make the sesame oil an outstanding salad oil.
On an average, two third sesame seeds of the worlds are processed into oil and meal (Kang et al., 2003).
The quality of the oil and variety of yield continue to raise (Bandyopadhyay and Ghosh, 2002). In
addition to using sesame oil for cooking foods, it may be used for nutraceutical food (Morris, 2002). In
2003, the reserved area for sesame planting in the world was 6.57 million hactares; with a production
rate of 3,096 million tonnes per year and an average yield of 471.2kg/ha (Ofosuhene et al., 2010). In
recent times, a nutraceutical diversity of sesame uses have been open to the elements from such as
sesamolin, assesamin, sesamol are lipidsoluble antioxidants and sesaminol, lignan glucosides and
sesame lignans are originate to be antioxidative and health benefiting. Sesame meal is a significant
protein resource for the utilization of mankind because of the presence of sulfur-containing AA. It has
protein content ranging from 45–55%. Sesamolin which is derived from seeds of sesame inhibit
expansion of leukemia cells in human (Bandyopadhyay and Ghosh, 2002).
The consumption of whole sesame seed shows the increase plasma γ-tocopherol and improved vitamin E
action, which is believed to reduce heart disease and cancer. Sesame oil is considered to satisfy
compound organ failure and boost endurance speed during endotoxemia in rats, while defending aligned
with lipopolysaccharidemotivated oxidative and influencing constructively the blood glucose,
7
glycosylated hemoglobin, antioxidant levels and lipid peroxidation in diabetic. Sesame intake also
affects confidently antioxidant status, blood lipids and sex hormones in postmenopausal women (Wu et
al., 2006).
Sesame is cultivated broadly from humid to moderate regions of the world. Sesame seeds contain
normally 25– 35% of protein and 55% of oil. The oil is rich in unsaturated fat. The richest fatty acids in
sesame oil are linoleic acid (37–42%) and oleic acid (41–45%) (Kang et al., 2000: Kim et al., 2002).
The effects of germination on the chemical composition and biochemical constituents of seeds differ to a
great degree with the plant kind, seed cultivars or varieties and the germination circumstances. Such
changes are important to the marketable applicability of sesame, more so if the health-improving
functional constituents are sought. Nevertheless, sesame in recent times recognized as a chief cause of
allergic reactions between infant and young children and a young woman that is amazing as sesame oil
is used widely in the cosmetic and pharmaceutical industries because of its apparently low antigenicity
(Caminiti et al., 2006). Allergens that belong to seed storage proteins, ordinary food allergens have been
recognized in sesame seeds. Therefore it is thus significant to check the protein level in sesame. As the
investigation of biochemical and chemical ingredients provided by germinated seeds leftovers deficient,
the benefits and limitations of germinating seeds utilized for human have not been recognized. To
maintain the advantageous level of sesame seeds for marketable utilizations, it is vital to outline their
compositional changes during and after germination
(Beyer et al., 2002).
Sesame is grown for its seeds and the primary use of the sesame seed is as a source of oil for cooking.
The young leaves may also be eaten in stews and the dried stems may be burnt as fuel with the ash used
for local soap making but such uses are entirely subordinate to seed production (Table 2.1). The crop of
sesame is commercialized in a number of forms. Most sesame seeds are processed directly into oil by
the grower or within the producing region but are also sold in various stages of processing, for various
uses, such as meal, paste, confections and bakery products (Salunkhe et al., 1991).
8
Table 1.1 Products of sesame and its uses
Part used
Seeds Products Description
Confectionery Fried seeds bound together with sugar syrup, whole seeds baked into
and Biscuits Biscuits, popular in northern Europe either incorporated into breads or
Seeds as decorative toppings, a paste of sesame seeds is used as an ingredient
in eastern Mediterranean and Middle Eastern foods
Oil Varied uses To treat ulcers and burns, low grade oil is used in making soaps, paints,
lubricants, and illuminants
Cake Food and feed Protein rich useful supplement, used in some Indian cooking
The Carbohydrates in sesame seed are composed of 3.2% glucose, 2.6% fructose and 0.2% sucrose
while the remaining quantity is dietary fibers. The nutrient composition of sesame seeds is enlisted in
Table 4 and 5. Also, they have desirable physiological effects including antioxidant activity, blood
pressure and serum lipid lowering potential as proven in experimental animals and humans (Sirato-
Yasumoto et al., 2001). The major protein fraction (globulin) in sesame contains about 95% of 13S
globulin and seems to be a simple, salt soluble, very susceptible to heat denaturation and similar in
subunit structure to soybean 11S globulin with more hydrophobic properties. The last property limits the
use of sesame proteins in certain food formulation, particularly in fluids and beverages, which indicates
the need to modify the functionality of sesame proteins before it can be used in processing of imitated
dairy products.
Sesamin Sesamolin
9
and limited in lysine and contains significant amounts of oxalic (2.5%) and phytic (5%) acids (Kapadia
et al., 2002).
Because oxalic acid is present in the hulls, decortication can remove most of it. Decorticated sesame
seeds have the following composition: 45-63% oil, 19-31% (averaging about 25%) proteins, about 14%
carbohydrates and about 3% ash. Unlike many oilseeds, sesame meal is devoid of anti-tryptic
compounds. Sesame oil is very rich in polyunsaturated fat used in margarine production and cooking
oils.
The valuable components of sesame seed are the oil and protein and the contents of these have been
determined for several varieties of sesame which were grown in the southern and southwestern
parts of the U.S. (10). Oil contents varied from 45-63% and averaged 54%. Protein contents varied
from 17-32% and averaged 26%. The average protein content of the oil-free meals was 57 (Williams,
2005).
Table 2.2 Nutrient composition of sesame seeds
10
2.5 Sesame oil description
Sesame oil is highly stable and rarely turns rancid in hot climates. It is rich in unsaturated fatty acids
where the fatty acids composition is 14% saturated, 39% mono-unsaturated, and 46% poly-unsaturated
fatty acids (Toma and Tabekhia, 1979).
Edible oils are resulting from plants and animals. Oils from plants are termed as vegetable oil. The
principal sources of vegetable oils are nearly plants, which include sunflower, soybeans, cotton seed,
groundnut, rapeseed, corn, melon and sesame seed. Other sources are oil bearing perennial plants such
as shear, olive, cashew coconut and palm. Sesame seed is rich in oil content with about 53% quality
edible oil, 42% cake and 5% moisture seed (Akinoso, 2006).
Sesame seed oil may be used directly exclusive of refining is an ordinary salad oil, which could need
small or no winterization and is one of the marginal vegetable oils. Clinical studies have shown that
sesame oil consumption has too many benefits to health like minimizing the occurrence of cancer,
contributes to the avoidance of degenerative processes; therefore decrease the death rate through cerebro
and cardio -vascular diseases. Health benefits of sesame, such as antioxidative, hypocholesteremic,
antihypertensive, immunoregulation and anticancer are mainly accredited to lignans and their glycosides
(Hany et al., 2000).
The level of oil of the sesame seeds ranges from 41.6 to 62.5%, the average being 53.2%. Sesame
contains nearly 85% unsaturated fatty acids. Seed contained 48.4% crude oil, 5.6% moisture, 20.2%
crude proteins, 7.69% carbohydrate (by difference) and 9.3% crude fiber. Mineral profile (mg/100g) of
seed is Calcium 415.38 ± 3.14, Phosphorus 647.25 ± 3.52, Potassium 851.35 ± 3.44, Magnesium 579.53
± 0.42 and Sodium 122.50 ± 4.21. Chemical study of cake extract of sesame showed 4.1% ash, 51.0%
fat, 19.7% sugar 6.8% protein and a total of 14.3% lignans and lignan glucosides (Nzikou et al., 2009).
Fatty acid profile of sesame oil showed that major component was linoleic acid containing 41.8–45.1%
of the total fatty acids, followed by stearic 32.6–24%, palmitic 8.2–7. %, oleic 4.6–5.6% and these four
comprised on 96% of the total fatty acids. About 83% of total means of linoleic and oleic acids were as
unsaturated fatty acids of sesame. Sesame oil fit for human consumption because high amount of
unsaturated fatty acids increases the quality of the oil. Saturated fatty acids of sesame oil were palmitic
and stearic acids with a range of 9.1–10.4 and 3.2– 5.9%. Phenolic compounds donate a hydrogen atom
o serve up as significant antioxidants because of their donating ability in order to form stable radical
11
intermediates. Hence, they phenolic compounds help in prevention the oxidation of different biological
molecules (Were et al., 2006).
Applied pressure, heating temperature, heating duration, moisture content, particle size, handling and
storage are factors influencing yield and quality of vegetable oil expression. The degree of influence
varies with kind of oilseeds and method of oil expression. Effects of some of these parameters on yield
and quality of oil expressed from sesame using expeller were studied. Moisture content, duration of heat
treatment and pre heating temperature were studied (Akinoso et al., 2006).
Moisture content has highest influence on sesame seed oil yield. To increase oil yield, moisture content
is reduced while roasting duration and roasting temperature are increased. Temperature has less effect
on increasing free fatty acid values while moisture may have a stronger effect. The hydrolysis of
meadow foam triglycerides improved as moisture level of the seeds would sustain. The free fatty acid
values of the oil samples show improvement with enhancing temperature and moisture. Optimum
condition was achieved at seed moisture content of
4.6% wet basis, roasting time and temperature of 13.0 minute and 124.2 0C respectively. At these
conditions, oil yield was 50.4% of substance, corresponding to 90.1% effectiveness of oil expressed.
Free fatty acid was 1.1% m/m while oil impurity was 0.1% and color rating was 6.2 lovibond units
(Mohammadzadeh et al., 2009).
Table 3.3 Amino acid and fatty acid composition in sesame seeds Source (Williams, 2005)
12
Palmitic acid (16:0) 11.7
Stearic acid (18:0) 0.52
Oleic acid (18:1) 41.4
Linoleic acid (18:2) 39.4
Linolenic acid (18:3) 0.4
Arachidic acid (20:0) 0.4
Behenic acid (22:0) 0.6
The high proportion of oil content in the seeds makes them feasible for commercial extraction. The oil
was found to be cyanide free, therefore appropriate for human utilization. The protein level for enzyme
isolated seeds being remarkably lower than that of solvent-isolated might be accredited to the removal of
protein in the aqueous stage as is evidenced by the occurrence of substantial amounts of protein (13.9–
25.7%) (Mohammed et al., 2007).
13
In extraction, successive washing of oleaginous material with solvent is performed until equilibrium is
reached or near equilibrium between the oil content of the solid and that of the solvent, i.e., when the
solvent absorbed by the solid and solvent in the free miscella containing the same amount of oil
dissolved. When this occurs, the miscella is drained and another washing takes place
The ability to extract an oil from an oilseed depends on the nature of the oil, the nature of the solvent,
the temperature and the contact time between solvent and grain mass, flake thickness and conditions of
pretreatment of the seeds. Attah & Ibemesi (1990) evaluated the solvent capacity and solvent effects in
the extraction of oils from four native plants. The following solvents were used: petroleum benzene (60-
80 o C), cyclohexane, isopropyl ether, ethyl acetate, tetra hydro furan, propan-2-ol and acetone. The
authors found that oil extraction performance of each solvent appears to be generally dependent on the
nature of the oil, i.e. ethyl acetate and tetra hydro furan gave the highest oil yields in rubber their oil
yields in melon gave next to lowest value. Hexane is used as a solvent to commercially extract oil from
rice bran. However, hexane poses potential fire, health, and environmental hazards. Short-chain
alcohols, especially ethanol and isopropanol, have been proposed as alternative extraction solvents due
to their greater safety and reduced probability of regulation. Alcohols tend to extract more nonglyceride
materials than hexane, due to their greater polarity. Typically, alcohol-extracted oils contain more
phosphatide and unsaponifiable compounds. Another important consideration was that solvent did not
affect the increase in the level of free fatty acid of extracted oils (17).
14
2.6.2 Supper critical extraction
The state of a substance is called supercritical fluid (SCF) when both temperature and pressure exceed
the critical point values, see figure 2.6
Extractions with supercritical fluid (SCF) solvents have emerged in recent years as highly
promising environmentally benign technologies for the production of natural extracts with high potency
of active ingredients colors, nutraceuticals or herbal medicines industries. Supercritical carbon
dioxide (SC CO2) at near desirable SCF solvent for extraction of natural products today as non-
flammable, and non-polluting. It’s near ideally suitable for thermally labile natural products. It is
generally regarded as safe (GRAS) and yields contamination-free, tailor enhanced shelf life. The
supercritical fluid extraction (SCFE) technique ensures high consistency and reliability in the quality
and safety of the bioactive heatit does not alter the delicate balance of bioactivity of natural
molecules. Mukhopadhyay, 2008)
Extraction using supercritical fluid, the oil produced has very high purity; however the operating and
investment cost is high.
Supercritical fluid extraction (SFE) eliminates the disadvantages of conventional solvent extraction
(CSE) which leads to degradation of heat sensitive compounds and leaves traces of toxic sol-vents in the
solute. This is a concern for food and medicinal extracts. By changing the operating pressure and/or
15
temperature, the low solubility of oil in supercritical fluids (SCFs) can be in-creased and also improves
the extraction rates. Therefore, new functional and/or nutritional characteristics for use in creating new
formulated foods can be improved using SFE. Extraction of oils from different seeds with supercritical
CO2 (scCO2) is widely re-ported (Özkal et al., 2005; Roy et al., 1996).
Extraction of sesame oil from sesame seeds using supercritical CO2 was carried out. The effect of
operating parameters such as pressure, temperature, and supercritical CO2 flow rate and particle size on
extraction yield were investigated. An increase in the pressure and the supercritical CO2 flow rate
improved the extraction yield and also shortened the extraction time. The extraction yield increased as
the particle size decreased depending on decreasing intra particle diffusion resistance.
Sesame oil has a mild odor and a pleasant taste and, as such, is a natural salad oil requiring little or no
winterization. It is used as a cooking oil, in shortening and margarine, as a soap fat, in pharmaceuticals
and as a synergist for insecticides. Sesame oil is very popular as cooking oil in many countries, and
more expensive than other vegetable oils (Hai and Wang, 2006; Budowsk and Markely, 1951). An
analysis of the operating cost of SFE indicated that use both of CO2 and entrainer is much less
expensive than CSE (Salgınet al., 2004).
The investigated conditions which would give maximum oil yield from raw sesame seeds by scCO2
extraction. They examined the effect of three parameters including pressure, temperature and co-solvent
concentration on extraction yield and also used Response Surface Methodology to analyze the
experimental data. They reported that the presence of 10 vol.% ethanol gave maximum yield of 89.40%
at 276 bar and 70 o C relative to yield obtained by Soxhlet extraction using hexane (Odabas and Balaban
2002).
The mathematical modeling of experimental data obtained in SFE has the objective of determining
parameters for process design, such as equipment dimensions, solvent flow rate, particle size, and the
characterization of SFE to enable the prediction of the viability of SFE processes on an industrial scale,
through the simulation of overall extraction curves (Machmudah et al., 2006). The distribution of the
natural materials within the solid structure affects the selection of models. Extractable materials easily
accessible on the surface of the solid matrix, adsorbed on the outer surface, located within pores, or
probably distributed within plant cell homogeneously. There are many mathematical models used for
extraction of solutes from natural matrices in the literature to correlate over-all extraction curves
16
(Hortaçsu, 2000). The authors are aware, there are no investigation reported in the literature
mathematical modeling of sesame oil extraction from raw seeds.
The mechanical expression of oil from oilseeds is the most common method used for the removal of oil
from oil-bearing materials. This method is economical for small and medium scale oil processors in the
developing countries (Singh et al.1984). Although the use of a hydraulic press during expression results
in lower oil removal efficiency, it is preferred to the screw press by small scale producers because of lower
initial and running costs. The amount of oil expressed using the hydraulic press is affected by the pre-
pressing and pressing conditions such as particle size, moisture content, heating temperature, heating time,
applied pressure, and pressing time (Khan and Hanna 1983). Steinbock (1948) explained, that with the
exception of very small sized seeds like sesame, reduction of oilseeds to flakes by rolling is essential with
the size and hardness of the seeds determining the number of stages for the flaking operation. Heating is
essential because it completes the breaking down of oil cell walls, lowers the viscosity of the oil to be
expelled, coagulates the protein in the meal, and adjusts the moisture content of the meal to the optimum
level for pressing (Ward 1976). Oil yield has been shown by several researchers to be affected by the
temperature and duration of heating (Ajibola et al. 1990; Fasina and Ajibola 1989; Sivakumaran et al.
1985; Singhet al. 1984).
High heating temperatures and long heating times may have negative effects on the quality of expressed
oil and cake residue (Anjou 1972; Ohlson 1976). It is therefore important to identify the optimal heat
treatment required for processing sesame seed.
The moisture content of oilseeds before pressing affects the yield and quality of oil expressed. Cloudy oil
is obtained from seeds with high moisture content. Therefore, moisture content adjustment of the seeds is
necessary before pressing. Vaughan (1970) explained that the effect of moisture content on expression
17
efficiency can be related to mucilage development in the outer epidermal cells of the seeds. The mucilage
coating can impede the flow of oil from the cotyledon tissue. High oil yields ranging between 37.0 and
39.6% were obtained from samples of conophor nut with post-heating moisture content between 8 and
10% (dry basis) (Fasina and Ajibola 1989), while maximum oil yields of about40% were obtained when
the moisture contents of melon seed samples were reduced by about 5% (dry basis) (Ajibola et al.1990).
Singh et al. (1984) observed that the moisture content of sunflower seed was the most significant factor
affecting the expression of oil from the seed.
An important parameter related to the pressing efficiency is the determination of residual oil in the cake.
High pressures can lead to cakes with less than 10% of oil content, which leads to higher crude oil
production. A reduction in speed of rotation of the shaft, for example, can reduce the oil yield, increasing
the oil content in the cake and solids in the oil (Jariene et al., 2008).
After pressing, the crude oil must be purified. A very common method of purification, especially for small
producers, is to allow the oil to stand undisturbed for a few days, removing the upper layer (purified oil)
and discard the bottom layer, consisting of fine pulp, water and resins. If this step is not enough, one can
filter the oil using a press filter or using a centrifuge, but both methods are costly (Bachmann, 2004).
In addition to obtaining the oil, mechanical expelling produces a very important by-product named cake
or meal. Some oilseeds cakes have high nutritional value and can be used as human food. Some are not
suitable as food, but serve to complement the diet of chickens, pigs and cattle. It is important to emphasize
the need for proper storage of seeds and cakes. They must be protected against the action of moisture,
rodents and insects. High moisture content will generate mold, which can alter the taste of cakes, being
rejected by the animals. Another problem is the development of mycotoxins such as aflatoxin, which in
high concentrations can be poisonous to humans and animals. (Bachmann, 2004).
18
In 1947, it was published a study evaluating the various types of solvents such as benzene, aviation
gasoline, methanol, ethanol, isopropanol, carbon disulfide, diethyl ether, ethylene dichloride, carbon
tetra chloride, trichloroethylene and the various petroleum naphtha. However, in 1947, the most
commonly used solvents in the United States were light paraffinic petroleum fractions, such as the
hexanes, heptane and pentanes. The hexane was finally chosen because of its ease to evaporate and left
no residual hateful odors or tastes. There are two types of hexane: normal, also known as n-hexane; and
commercial, named extraction-grade hexane. The n-hexane is pure and boils at 69 o C, while the
extraction-grade hexane is not pure. So, the boiling temperature could be slight higher or lower than 69
o
C.
2.7.2 Extractor Temperature
As the temperature of the miscella increases, its rate of diffusivity through the cell walls of the
oleaginous material increases. As the prepared oleaginous material/ oil contained seed/ enters the
extractor at approximately 60 o C, and both the oil and meal fractions are heated in excess of 100 o C in
subsequent process steps, there is no extra thermal energy required for operating the extractor at a warm
temperature. As a result, optimizing extraction results requires operating the extractor as warm as
possible.
There is an upper limit for the extractor operating temperature. The solvent must remain safely in a
liquid state. As the boiling range of commercial hexane is typically 64–69 o C at sea level, the maximum
possible temperature to prevent boiling is 63 o C. operating on the edge of the boiling range could cause
rapid evaporation during an upset condition. Rapid evaporation can cause pressurization of the extractor,
leading to excessive solvent loss, a safety hazard. Therefore, most processors operate the extractor at 60
o
C to provide several degrees of safety margin below the lower end of the solvent boiling range.
If the prepared material temperature is too low, or heat loss in the extractor is too high, then it may not
be possible to achieve an extractor temperature of 60 o C. The materails should be heating to the
temperature close to extraction temperature. It is necessary to ensure additional contact time between
solvenet the soil seed flakes is provided to achieve desired results. The size of the extractor is
proporational to contact. However, by insulating the conveying system and extractor, the heat loss can
be prevented and operation can be maintained at 60 o C. This helps to reduce the capital cost of the
extractor, avoiding oversizing the extractor to compensate for low operating temperature.
19
2.7.3 Extraction Time
The total time that the oleaginous material spends in the extractor is residence time. Residence time can
be subdivided into wash time and drain time. Wash time is the time the oleaginous material spends
under the washing nozzles of the extractor, and drain time is the time the oleaginous material spends
draining prior to discharge.
Wash time can be further subdivided into contact time and dormant time. Contact time is the time a
particle of oleaginous material spends in the washing zone of the extractor where the particle is in
contact with miscella. Extraction only takes place during contact time. Dormant time is the time a
particle of oleaginous material spends in the washing zone of the extractor where it is not in contact with
miscella. The ratio of contact time to dormant time varies with extractor design.
Extractors with deep material bed depth and small bed surface area are generally operated by immersing
the oleaginous materials in miscella. This is accomplished by providing a sufficient miscella flow rate
per unit of material bed surface area to ensure that miscella fills all of the voids around the oleaginous
material particles as it passes down through the material bed. This type of extractor operation provides a
very high ratio of contact time to dormant time in the washing zone.
Extractors with shallow bed depth and large bed surface area are generally operated by percolating the
miscella down through the oleaginous materials. With most oleaginous materials, the oleaginous
material particles occupy 40% to 50% of the material bed and 50% to 60% of the material bed is
composed of void spaces between the particles. In percolation, the oleaginous material particles are
surrounded by both solvent vapor and miscella as the miscella rains downward.
2.7.4 Flakes Size (particle size)
Various oleaginous materials are prepared for extraction using different process steps, but with virtually
all oleaginous materials, one process step is flaking. The principle purpose of flaking is to reduce the
thickness of the oleaginous material to reduce the distance and number of cell walls that miscella needs
to diffuse through to reach the oil bodies. Note that for soybeans, a typical 0.38-mm-thick flake is
approximately 20 cells thick. By reducing the particle thickness, the time required for miscella within
the cellular structure of the oleaginous material to reach equilibrium with the miscella surrounding the
oleaginous material is reduced. By reducing particle thickness, desired results can be achieved with less
contact time. If all other extraction parameters remain constant, reduced particle thickness will allow a
smaller extractor to be used.
20
Reducing the particle thickness represents additional cost. For example, on soybeans, reducing particle
thickness from 0.38 mm down to 0.30 mm will increase flaking mill electricity requirements by 1 to 2
kwh/ton of soybeans processed. As this is a significant ongoing operating expense, it is not
economically feasible to undersize an extractor and reduce particle thickness. Conversely, by increasing
particle thickness, desired results will demand more contact time. An extractor can be oversized to
obtain desired results with increased particle thickness, thereby reducing ongoing operating cost.
For all oleaginous materials, the economic balance between the initial cost of the extractor and the
ongoing electricity costs required for flaking can be analyzed and the optimum particle thickness can be
determined.
21
The production of gums and soaps stock in integrated crushing refining is a process of continuously
removing the gums and free fatty acids from the oils and continuously adding these as gums or soap
stock to the meal or expellers. The components in the soap stock are part of the natural composition of
seeds or beans. This means that only natural components separated from the seeds and beans are
returned back into the crushing process. Whether integrated crushing refining plants add soap stocks
back to the meal or expellers is determined by the design of the facility. It is not subject to daily
management decisions. In their meeting on 17 and 18 January 2013, the Standing Committee on the
Food Chain and Animal Health, section Animal Nutrition confirmed the feed material status of meals
and expellers to which soap stocks have been added in integrated crushing and refining plants.
2.8.4 Winterization
Optionally both chemical and physical refining during winterization waxes are crystallized and removed
in a filtering process to avoid clouding of the liquid fraction at cooler temperatures. The filter cake that
remains after the filtering process consists of oil, waxes and filter aid. The filter cake can be recycled to
the toaster and added to the meal (in an integrated crushing/refining plant) or sold as such as a feed
material (refining standalone). The term winterization was originally applied decades ago when
cottonseed oil was subjected to winter temperatures to accomplish this process. Winterization processes
using temperature to control crystallization are carried out on sunflower and maize oil. This process is
also referred to as dewaxing.
22
2.9 Minor Components of Sesame Oil
Many of the special properties of sesame oil are due to the presence of 0.4-1.1% sesamin, 0.3-0.6%
sesamolin and traces of sesamol in the oil (4, 18). As shown in Figure 2.3. Sesamin and sesamolin
have the same 2,7-dioxabicyclo- (3,3,0)-octane nucleus and both have two 3,4-methylene
dioxyphenyt substituents. In sesamin these are attached directly to the nucleus, while in sesamolin
one is attached directly and the other through a connecting oxygen atom. Sesamol is the free 3, 4-
methylenedioxyphenol. Thus sesa- molin is an acetat-type derivative of sesamot. The absolute
configurations of sesamin and two other sterioisomers are known (17).
The superior oxidative stability of sesame oil relative to other oils is largely due to sesamol, which is
usually present in traces but may be released from sesamolin by hydrogena- tion, by acid or acid
bleaching earths or other conditions of processing or storage. Sesamol may also be removed by some
bleaching earths or by deodorization. The effectiveness of sesamol as an antioxidant on the keeping
quality of lard has been reported (20).
It was more effective than butylated hydroxytotuene (BHT), butylated hydroxyanisole (BHA) and
several other antioxi- dants and was surpassed only by propyl gallate. In a more recent study of
antioxidants (21), the induction period for autoxidation of methyl octadecadienoates, in the presence of
0.01% of various antioxidants, was estimated by measuring the time for pickup of a certain weight of
oxygen. In the natural cis, cislinoleate, sesamol was more effective than BHT or BHA and was
surpassed only by propyl gallate. Sesamol was not effective in the Trans, trans-ester. In the conjugated
ester, BHT, BHA and sesamol were equally effective and were more effective than propyl gallate.
23
Sesame oil may be readily detected in mixtures with other oils by tests for sesamol, sesamolin and
sesamin. For this reason it has been used in some countries as a marker in margarine and other
hydrogenated oils. The analyses by the Villavecchia and other color tests, by UV spectrometry and by
thin layer chromatography have been thoroughly reviewed (16).
The sterols and triterpenes in sesame oil have been separated and identified using thin layer and
gas liquid chromatography (18). The 0.19% of sterols are the usual plant sterols and are, in order of
decreasing concentration, fl-sitosterol, campesterol and stigmasterol. The 0.03% of triterpenes includes
at least six compounds, three of which were identified as cycloartenol, 24-methylenecycloartanol and
c~-amyrin (23).
Sesame oil has a high percentage of polyunsaturated fatty acids (omega-6-fay acids) but keeps at room
temperature uniquely due to the presence of sesamol and sesamin, two naturally-occurring preservatives.
The presence of high polyunsaturated fatty acids content make it possible to use sesame oil for cooking
24
in place of other edible oils and to help reduce high blood pressure and lower the amount of medication
needed to control hypertension. Sesame oil can also be used for medicinal purposes which include
reduction of cholesterol levels, anti-bacterial effects, and even slowing down certain types of cancer
(www.nutrition-and-you). Apart from these various constituents present in the sesame oil have anti-
oxidant and anti-depressant properties. Sesame oil enhances many dishes including salads, pasta, sauces
and other hot and cold food as well as sweet dishes, the manufacture of cosmetics such as soap, hair
conditioners, and bath oil. The cake obtained after expression can be used in the preparation of livestock
feed. The oil has a neutral taste and significantly improves nutritional value (www.nutrition-and-you).
25
Chapter Three
Sesame seed sourced from Hummera harvested in 2016, which bought at Merkato Addis Ababa
Ethiopia.
Solvent n-Hexane were used for extraction process, which bought from Neway Chemicals sale and
distruster. Activated carbon used for the purpose of for color absorbent, which bought from Neway
Chemicals sale and distruster. Caustic soda, which bought at Neway Chemical distruster.
Addis Ababa Instate of Technology provide such equipment Soxhlat extractor were used for extraction,
Beaker to measure chemical and water, jar, water bath, Thermostatic water bath. Balance simple
electronic mass balance from AAiT. Oven which owned by AAiT works about 120 oc. Measuring
cylinder, etc.
Sample analysis
20g, 30g, and 40g of the cleaned sample was weighed and dried in an oven at 100°C and the
weight was measured every 2hrs. The procedure was repeated until a constant weight was obtained.
The percentage moisture in the kernel was calculated using the following:
(w1−w2)∗100
moisture content = (3.1)
w2∗100
26
3.2 Methods
Extraction using solvent has several advantages. It give higher yield and less turbid oil than mechanical
extraction, and relative low operating cost compared with supercritical fluid extraction.
The laboratory procedure that can be followed for the extraction sesame oil using soxhlate extractor was
as follows.
Raw material
Cleaning &Measuring
Drying oven
Hexane
Solvent recovery
Oil
Figure 3.1 process flow sheet
The raw material was bought from Merkato Addis ababa Ethiopia, after had the raw material further
cleaning sesame seed to remove foreign matter and measuring using electronic balance. Drying seed
using oven to have 6-10 % moisture content and put the sample put in desiccator. Crushing the seed to
lower the size Oil extraction using soxhlate and cold press machine.
27
3.2.1 Soxhlet extraction
The experimental procedure was done in AAIT Chemical Engineering Laboratory. Each of the
experimental run was designed with the aid of Design Expert using the central composite design of the
response surface methodology. The sesame seed (20 g per sample) was packed inside a thimble bag
(see Figure 3) and placed inside the thimble chamber of the 100 ml Soxhlet extractor shown in
Figure 4. The extractor itself was placed inside a thermostatic water bath (shown in Figure 5). A round
bottom flask containing n-hexane as well as a condenser was fixed to the extractor. The flask was heated
to a temperature above the boiling point of the solvent as indicated in the design matrix. The solvent
then vaporized and passed through the prepared seed to remove its oil. The mixture obtained
(solvent and oil) moved directly into the round bottom flask. The process was allowed to continue
for the specified time, as obtained from the experimental design. Thereafter, the oil extracted was
recovered by distilling the solvent using the same apparatus.
28
Figure 3.3 Soxhlet Extractor
29
Figure 3.5 laboratory setup of Soxhlet extraction
30
3.3 Characterization of sesame oil
3.3.1 Determination iodine value
Add 40ml of cyclohexane and 40ml of acetic acid glacial. Weight the required amount of 0.3646 gm. of
oil
Add 15 ml of mixture of cyclohexane and acetic acid glacial and Add 25 ml of weji’s solution keep 1 hr.
of reaction to dark place. Add 20 ml of potassium iodide to the solution. Add 150 ml of distilled water
and titrate by using sodium thiosulphate.
1.269(Vblank − Vsamle)
IV =
mass of oil
V blank= 40 ml
V sample=10 ml
Mass of oil = 0.4636 gm.
1.269(40 − 10)
IV =
0.4636
IV = 82.11ml/gm
31
N is concentration of ethanolic KOH
Acid value = 0.42 mg KOH/g
3.3.3 Gas Chromatography mass spectroscopy (GC/MS) result analysis
The Free fatty Acid value was determined from GC/MS analysis using the area covered under the peak
graph as follow.
From table 3.1 the composition of sesame oil obtained from GC/MS analysis were found 10.79% palmic
acid methyl ester, 57.55% linoleic acid, 27.101 oleic acid and 4.55% stearic acid methyl ester.
32
3.3.4 Determination of density
Measuring of the density of oil was carried out using picnometer that 50cm 3
mass of oil
density =
volume of oil
45.6 gm
density =
50 cm3
density = 0.912 gm/cm3
Variable Levels
Minimum(-1) Maximum(+1)
Moisture content (%) 6 10
Temperature (o C) 73 83
Extraction Time (Hr.) 5 7
After obtaining the responses (oil yield) from each of the experiments, the values (the responses) were
entered into the appropriate column in Design Expert, and the response together with the factors
33
considered were analyzed, and a quadratic and a cubic models relating the percentage oil yield to the
factors considered were developed for the extraction. In order to get a model that would best fit the
experimental results and take care of effects of all the factors, the developed models were modified. The
modifications carried out resulted in improvements in the performances of the models. Using the
quadratic models, a numerical optimization was carried out and the optimum conditions of the three
factors investigated for the extraction were obtained. For the quadratic model, the goals for the factors
were in a range while that of the response was “maximize”. In maximizing the response using cubic
model, the goal of each of the factors was a target of moisture content 6%, extraction temperature of 83 o
C and extraction time of 7 hr were found to be the optimum operating conditions, which led to optimum
oil yield of 50.17 % for quadratic models.
34
Chapter four
Result and discussion
4.1 soxhlate extraction yield data
The experiments were carried as per the experimental design. The data generated from the experiment
are given in the Table 4.1.
As shown in table 4.1, the result optaind showed that moisture content and extraction time affected the
oil yield most. For instance, looking at run 13 and run 9 in which the moisture content increased from
6% to 10% oil yield was noted to decrease from 50.2 % to 47.43%. However, comparing. Run 1 with
Run 13, similar variation in extraction time led to increase in oil yield from 45.83 to 50.2%. Although,
comparing the extraction temperature run 14 and run 1 in this manner also oil yield incresed from 43.19
to 45.83%.
After the results of the experiments were obtained and considered, they were, first, used to develop a
quadratic model equation for the extraction. The developed quadratic model equation is as shown in
Equation (2) while the analysis of variance (ANOVA) of the model is given in Table 3.
Yield of Oil = +45.71 + 1.58 ∗ A + 1.64 ∗ B − 1.04 ∗ C + 0.38 ∗ A ∗ B − 0.14 ∗ A ∗ C−
0.16 ∗ B ∗ C + 0.17 ∗ A − 0.63 ∗ C2 (4.1)
35
Table 4.1 The central composite design matrix and responses
Moisture
Run Temperature(oC) Time (Hr.) cntent (%) Yield of oil
A B C %
1 83.00 5.00 6.00 45.83
2 78.00 6.00 8.00 45.85
3 78.00 6.00 8.00 45.5
4 78.00 6.00 11.36 42.28
5 78.00 6.00 8.00 45.81
6 78.00 7.68 8.00 48.5
7 73.00 7.00 10.00 43.83
8 86.41 6.00 8.00 48.9
9 83.00 7.00 10.00 47.43
10 73.00 5.00 10.00 41.62
11 78.00 6.00 8.00 45.62
12 78.00 6.00 8.00 45.66
13 83.00 7.00 6.00 50.2
14 73.00 5.00 6.00 43.19
15 69.59 6.00 8.00 43.5
16 78.00 6.00 4.64 45.58
17 83.00 5.00 10.00 43.72
18 78.00 6.00 8.00 45.72
19 73.00 7.00 6.00 46.04
20 78.00 4.32 8.00 43.031
The coefficients in the model are determined using quadratic regression using ANOVA analysis
software. The coefficients obtained is inserted in the equation. The ANOVA is used to deterime sum of
squares, mean square, F-value, p-value, and other relevant parameters. The result obtained from the
analysis is presented in Table 4.2.
The Model F-value is 963.18 which implies the model is significant. According to the F-value, there is
only a 0.01% chance that a "Model F-Value" this large could occur due to noise.
36
Values of "Prob > F" less than 0.0500 indicate model terms are significant. In this case A, B, C, AB,
AC, BC, A2, C2 are significant model terms. According to litertaure, values greater than 0.1000 indicate
the model terms are not significant. If there are many insignificant model terms (not counting those
required to support hierarchy), model reduction may improve your model.
The "Lack of Fit F-value" of 0.51 implies the Lack of Fit is not significant relative to the pure
error. There is a 78.09% chance that a "Lack of Fit F-value" this large could occur due
to noise. Non-significant lack of fit is good we want the model to fit.
Std. Dev. 0.11 R-Squared 0.9986
Mean 45.39 Adj R-Squared 0.9975
C.V. % 0.24 Pred R-Squared 0.9955
PRESS 0.42 Adeq Precision 115.185
Table 4.2 ANOVA for Response Surface Reduced Quadratic Model
Sum of Mean F p-value
Source Squares df Square Value Prob > F
Model 93.53 8 11.69 963.18 < 0.0001 significant
A-Temperature 34.11 1 34.11 2809.81 < 0.0001
B-Time 36.54 1 36.54 3010.11 < 0.0001
C-mositure 14.79 1 14.79 1218.12 < 0.0001
content
AB 1.14 1 1.14 93.92 < 0.0001
AC 0.15 1 0.15 12.46 0.0047
BC 0.21 1 0.21 17.40 0.0016
A2 0.41 1 0.41 34.09 0.0001
C2 5.85 1 5.85 481.93 < 0.0001
Residual 0.13 11 0.012
Lack of Fit 0.051 6 8.464E- 0.51 0.7809 not significant
003
Pure Error 0.083 5 0.017
Cor Total 93.66 19
37
4.1.1 Effect of temperature on oil yield
The quantity of oil can be affected by temperature. From the data generated in the expereiment, the
effect of temeperature on oil yieald is ploted in Figure 10. . The plot shows thatincreasing temperature
raised oil yield. Based on the findings, the yield was found to be enhanced with increasing
temperature. This was because of rising the temperature enhancedboth the diffusion coefficient and the
solubility of the oil in to both solvents, Thus heat treatment improves the extraction sesame oil.
The higher extraction temperatures the easier to break the molecule inside the seed; as a result,
the yield also gets high.
Design Points
X1 = A: Temperature
48.05
Actual Factors
B: Time = 6.00
C: mositure content = 8.00
Yield of Oil
45.9 2
2
43.75
41.6
A: Temperature
38
4.1.2 Effects of Extraction Time on oil yield
Extraction time is one of the factors that affects the percent yield of sesame oil. . The experiemntal
result shows extraction time influences greatly the percentage yield of sesame oil using n-hexane as a
solvent. This is shown Figures 11. The plot shows the increase in the contact time increased the oil yield
till transfer of oil from the kernel powder to the solvent attains zero. In other word, when the maximum
amount of extractable oil is obtained, the oil yield level remains invariable even by extending the
extraction time. As shown in Figure 4.2, extracting the oil beyond six hours is wasting time because
using n-hexane as a solvent can find maximum yield at this time.
The Figure also shows the extraction rate is fast at the beginning of the extraction but gets slow
gradually. The reason is that when the kernel powder is exposed to the fresh solvent, the free oil on the
surface of seeds is solubilized and oil gets extracted quickly inducing a fast increase in the
extraction rate. Furthermore, since the oil concentration is low in the solvent at the beginning of the
extraction process, the oil diffuses quickly from the kernel to the liquid phase due to the
difference in concentration (driving force) of the oil. As the time passing by, the concentration of oil
increases in the solvent resulting in a decrease in the diffusion rate.
Design Points
X1 = B: Time
48.05
Actual Factors
A: Temperature = 78.00
C: mositure content = 8.00
Yield of Oil
45.9 2
2
43.75
41.6
B: Time
39
4.1.3 Effects of moisture content on oil yield
The effect of moisture content is shown in Figure 4.3. The plot shows that as the moisture content
decrease from 12% to 6%, the oil yield increased from 42% to 47%. In order to enhance the downstream
unit operation of flaking, oleaginous materials are typically heated in the range of 90 –110 o C
temperature. By heating and softening the oleaginous materials, it enables the oleaginous material to
stretch and flatten in the flaking operation with a minimum of fragmented particles being created.
For oleaginous materials being prepressed prior to solvent extraction, they are typically heated in the
range of 90 –110 o C temperature to decrease the viscosity of the oil and allow the prepress to expel the
oil and make a good quality cake
Design Points
X1 = C: mositure content
48.05
Actual Factors
A: Temperature = 78.00
B: Time = 6.00
Yield of Oil
45.9 2
2
43.75
41.6
C: mositure content
40
Design-Expert® Softw are
Yield of Oil
50.2
41.62
49.5
X1 = A: Temperature
X2 = B: Time
47.875
Actual Factor
C: mositure content = 8.00
Yield of Oil
46.25
44.625
43
7.00 83.00
6.50 80.50
6.00 78.00
5.50 75.50
B: Time A: Temperature
5.00 73.00
Figure 4.4 3D surface plot for effect of extraction time and extraction temperature on oil
yield
As Shown in Figures 4.4, the variations of extraction time and extraction temperature with oil yield
for the quadratic models. According to the figures, it was discovered that the variation of ettraction
time with temperature affecte oil yield.
41
Design-Expert® Softw are
10.00
Yield of Oil
Yield of Oil
Design Points 43.6338
50.2
41.62
9.00 44.5078
C: mositure content
X1 = A: Temperature 45.3819
X2 = C: mositure content
46.256
Actual Factor 8.00 6
B: Time = 6.00
47.1301
7.00
6.00
73.00 75.50 78.00 80.50 83.00
A: Temperature
Figure 4.5 Contour plot for effect of moisture content and extraction temperature on oil yield
Looking at Figures 4.5 and 4.6, the effects of the three factors (moisture content, extraction temperature
and extraction time) considered on the oil yield can be easily seen. From these figures, it can be seen
that the variation of moisture content was found to significantly affect the oil yield obtained from
sesame seed as the extraction time was varied. For instance, increasing the moisture content while
slightly varying the extraction temperature and extraction time as shown in Figures 4.5 and 4.6 led to
decrease in oil yield. That means, the oil yield was not significantly affected by the interaction of
temperature and extraction time as the moisture content is increase. So, it seems that the moisture
content should be controlled or reduced as much as possible to get the positive effect of temperature and
extraction time.
42
Design-Expert® Softw are
10.00
Yield of Oil
Yield of Oil
Design Points 43.453
50.2
41.62
9.00
44.3454
C: mositure content
X1 = B: Time 45.2377
X2 = C: mositure content
46.13
Actual Factor 8.00 6
A: Temperature = 78.00
47.0223
7.00
6.00
5.00 5.50 6.00 6.50 7.00
B: Time
Figure 4.6 Contour plot for effect of Time and moisture content on oil yield based on quadratic model
43
Design-Expert® Softw are
Expert® Softw are
7.00
Yield of Oil Interaction
Yield of Oil B: Time
Oil 50.2
gn Points
48.3984
Design Points
B- 5.000
2 B+ 7.000
6.50 47.3264 48.05
X1 = A: Temperature
Temperature X2 = B: Time
Yield of Oil
Time 46.2544
B: Time
43.75
5.50
44.1105
41.6
A: Temperature
Figure 4.7 Contour plot for effect of temperature and extraction time on oil yield on quadratic model
From the numerical analysis carried out for the quadratic model developed for oil extraction from
sesame seed, moisture content 6%, extraction temperature of 83 o C and extraction time of 7 hr. were
found to be the optimum operating conditions, which led to optimum oil yield of 50.17 % for quadratic
models. Furthermore, using the optimum parameters obtained from the response surface methodology
employed carried out to perform a validation experiment, oil yield of 50.17 % was obtained. The value
obtained was found to compare well with the predicted optimum yield. Therefore, the result obtained
has revealed that the optimum values of the parameters given by response surface methodology
with the aid of Design Expert were valid ones.
44
Diagnostics
The following figure 4.8. shows the relation between the actual value of the experiment and the
value predicted by the model equation developed by the Design Expert software.
48.05
Predicted
45.90
43.75
41.60
Actual
45
Chapter 5
5.2 Recommendation
The following recommendations are made on the subject area of sesame seed extraction:
Here in the experimental work, the solvent to solid ratio and seed particle size has not been studied. This
is due to. So, further investigation needs to analize the oil yield
Further plant design and economics analysis will also needs to be work for feature investigation on the
continuation of thesis paper.
46
References
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Department of Agriculture and Bio resource Engineering, University of Saskatchewan, Saskatoon, 1997.
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14. Ohlson, J.S.R. 1976. Processing effects on oil quality. Journal of the American Oil ChemistsSociety
15. P. J. Wan and P. J. Wakelyn, Technology and Solvents for Extracting Oilseeds and Nonpetroleum Oils ,
AOCS Press, Champaign, Illinois, 1997, pp. 14–18.
16. Pominski, J., H.M. Pearce and J.S. Spadero. 1970. Partiallydefatted peanuts - factors affecting oil removal
during pressing. FoodTechnology24 (6):92-94. Singh, M.S., A. Farsaie,L.E. Stewart and L.W.
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1991.
48
Appendix
Appendix A Integration Peak Area from Gas chromatography
spectrometer
49
50
Name Synonymous
Palmic acid Hexadecanoic acid
Methyl oleate 9-octadecenoic acid(z)
methyl ester
Lineolic acid 9-12 octadecadienoic acid
Stearic acid Methyl stearate
51
52
53