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Comparative Extraction of Some Non-Conventional Oil Seeds (Pentaclethra Macrophylla Benth) Using Different Solvents

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International Journal of Engineering and Technical Research (IJETR)

ISSN: 2321-0869, Volume-2, Issue-9, September 2014

Comparative Extraction of Some Non-


Conventional Oil Seeds (Pentaclethra Macrophylla
Benth) Using Different Solvents
Okpo S.O., Evbuomwan, B. O.
to as oil seeds. Conventional oilseeds are class of plants in
Abstract Comparative extraction of some which relatively large amount of lipids are stored in the seed
non-conventional oil seeds (Pentaclethra macrophylla benth) tissue [2].There are wide varieties of seeds and nuts that can
using n-hexane and ethanol have been investigated. Extraction produce oils for food, pharmaceuticals, skincare products,
parameters such as time, particle size and volume of solvent
aromatherapies, fuels and industrial lubricants. Also, some of
were varied and statistically analyzed. Also, the physicochemical
properties of the oil extracted were studied in order to compare
these plant derived oils can be used to make soap, body and
the extraction efficiency of the two solvents. The results of the hair oils, detergents and paint. Vegetable oils derived from
physicochemical properties for n-hexane and ethanol are as plant seeds have been playing vital roles to provide comfort in
follows; colour: raw sienne (dark brown) and raw umber (light human lives in various aspects. Outside the realm of food
brown), Density: 0.918g/cm3 and 0.921g/cm3 , melting point: 48 manufacture, vegetable oils also feature in a variety of
0
C and 470C, Saponification value: 152.72 mg/KOH/g and industrial uses ranging from the manufacturing of soap to the
164.39 mg/KOH/g, iodine value: 52.51 mg/KOH/g and 49.95 production of lubricants ,varnishes , plastics and paints. For
mg/KOH/g , acid value: 5.84% and 6.40% , free fatty acid value: instance, they have been used for illumination and lubricating
2.92 % and 3.20% , refractive index: 1.453 and 1.466 at 25 0C
purpose, production of detergents and cosmetics and for
and pH: 6.10 and 7.14, viscosity: 0.9100 and 0.9013 respectively.
The coefficient of determination (R2) value obtained from
coatings and paint for many centuries before an abundant and
ANOVA showed that ethanol is a good alternative solvent to cheap supply of mineral oil became available.
n-hexane. Nigeria, as a tropical country, has a wide variety of domestic
plants that produce oil-bearing seeds of sufficient volume
Index Terms Extraction, Oil seeds, Solvent, potential; for example, edible seeds like soya bean, peanuts,
Physicochemical and Anova and corn. According to [3], Nigeria has one of the most
extensive flora in continental Africa. Unfortunately, the vast
majority of the seed oils have not been adequately study and
characterized. A lot of work has been carried out on analysis
I. INTRODUCTION of seed Oils by a number of researchers, primarily because of
Generally, oils and fats from seeds and nuts constitute an extensive demands for oils both for human consumption and
essential part of mans diet. Fats and oils, together with for industrial applications; consequently there is an increasing
proteins, carbohydrates, vitamins and minerals, are the main need to search for oils from non-conventional sources to
nutrients required by the human body. Fats and oils are rich augment the available ones and also to meet specific
sources of energy, containing two and a half times the calories applications. Among these non-conventional oil seeds
of carbohydrates (per unit weight). In addition to being a includes Pentaclethra macrophylla benth (African oil bean
source of vitamins A, D, E and K, fats and oils also contain seed), African star apple, African pear, vine rubber etc.
essential fatty acids. These essential fatty acids are not Therefore, it is worth while to carried out extraction of oil
manufactured by the body and must be obtained from diets, from some nonconventional oil seed such as African oil bean
with linoleic, oleic and linolenic acids as examples of seed.
unsaturated fatty acids . However, continuous exploration and extraction of oils from
Vegetable oils are essential in meeting nutritional demands of the non conventional oil seeds is expected to check the
the globe and are utilized for many food and industrial expensive prices of the conventional oils thus making them
purposes .Plant seeds have been used since antiquity as affordable to people, most especially in the developing
sources of vegetable oil. Examples of some plant seeds which countries [4].This work seek to compare the effects of
have been conventionally exploited commercially for this different solvents on non-convectional oil seed (Pentacletra
purpose includes soybeans, cotton seed, groundnut, corn, Macrophylla).
palm seeds and sunflower [1]. These conventional sources of
vegetable oil are unable to meet the ever increasing demands
of domestic and industrial sectors. Fixed oil derived from
plants are usually obtained from plant seeds generally referred II. MATERIALS AND METHOD

A. Materials
Manuscript received September 10, 2014. Pentaclethra macrophylla benth used for this work were
Okpo S.O., Faculty of Process and Energy Systems Engineering,
Department of Chemical Engineering, University of Port Harcourt, Port
obtained from Ozoro market in Isoko North Local
Harcourt, Rivers State, Nigeria. Government Area of Delta State of Nigeria.
Evbuomwan, B. O., corresponding author

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Comparative Extraction Of Some Non-Conventional Oil Seeds (Pentaclethra Macrophylla Benth) Using Different
Solvents

The solvents used were n- hexane and ethanol. All chemical experiment and the extraction was carried out for a given (set)
used were of analytical grade and supply were made by time. After the extraction with solvent, the set up (Soxhlet
Science Laboratory Technology Department of Delta State extractor) was dismantled and the miscella (mixture of solvent
Polytechnic, Ozoro,.Nigeria and extracted oil) obtained was poured into evaporation dish
and placed on the heating mantle. The heating mantle was set
at 78oC and 68oC for ethanol and n-hexane which is their
B. Preparation of sample
boiling point respectively , so that , the solvent is brought to
The sample seeds were thoroughly washed and seed coat were the vaporization point. After evaporation process, the weight
removed with sharp knife, the embryo( endoderm) were sliced of the oil was determined. This procedure was repeated for
into smaller pieces and dried in an oven at a temperature of ethanol and n-hexane.for different experimental conditions.
about 1050C - 1100C. After cooling ,the sliced dried seeds The oil extract was Characterized for the determination of oil
were ground using a manual grinding machine and sieved quality by ASTM and AOCS(1993) methods.
through five different laboratory sets of sieves to obtain
particle sizes of 0.85mm, 1.18mm, 2.36mm, 3.35mm and
6.70mm. The samples were stored in separate air tight III. RESULTS AND DISCUSSIONS
containers and labeled adequately
C. Procedure A. RESULTS
A known mass (say 20g) of milled sample of African oil been The results of the physico-chemical properties of the
seed was weigh with Setra analytical weighing balance with extracted oil for both solvents is presented in table 4.. Tables,
model number BL- 410s and placed in the thimble of the 4.2, 4.3, 4.4 and figures 4.1, 4.2 and 4.3 presents result on the
Soxhlet extractor. A determined quantity of solvent was filled effects of particle size on oil yield, effects of time on oil yield
into the thimble of 250 ml Shuniu GG-17 Soxhlet extractor. and effects of solvent volume on oil yield respectively.
The heating mantle was set at a specified temperature for the

TABLE 4.1: PHYSICO-CHEMICAL PROPERTIES OF PENTACLETHRA MACROPHYLLA BENTH


OILEXTRACTED WITH ETHANOL AND N-HEXANE
SOLVENTS
EXTRACTED OIL PROPERTIES ETHANOL N-HEXANE
Refractive index ( 250C) 1.453 1.466
Melting point (0C) 48oC 47oC
3
Density (g/cm ) 0.918 0.921
Viscosity (cP) 0.9100 0.9013
pH Value 6.10 7.14
Colour Raw sienne(dark brown) Raw umber (light brown)
Saponification value (meq/KOH/g) 152.72 164.39
Acid value (mg/KOH/g) 5.84 6.40
Iodine value (mg/100g of sample) 53.19 76.4
Free fatty acid (mg/KOH/g) 2.92 3.20

TABLE 4.2: EFFECTS OF PARTICLE SIZE ON OIL YIELDS


Extraction With N-Hexane Extraction With Ethanol
S/N
Particle Size Mass of Oil % Oil Yield Mass of Oil % Oil Yield
(mm) Extracted (g) Extracted (g)
1. 0.85 8.412 42.06 6.502 32.51
2. 1.18 7.800 39.00 6.105 30.53
3. 2.36 6.350 31.75 5.509 27.55
4. 3.35 6.088 30.45 5.157 25.79
5. 6.70 4.490 22.45 3.846 19.23
TABLE 4.3: EFFECTS OF TIME ON OIL YIELDS
Extraction With N-Hexane Extraction With Ethanol
S/N Mass of Oil Mass of Oil
TIME (min.) % Oil Yield % Oil Yield
Extracted (g) Extracted (g)
1. 20 7.003 35.02 5.912 29.56
2. 30 8.328 41.64 6.661 33.31
3. 40 8.566 42.83 6.793 33.97
4. 50 8.602 43.01 8.280 41.40
5. 60 8.763 43.82 8.824 44.12

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International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-9, September 2014

TABLE 4.4: EFFECTS OF VOLUME OF SOLVENT ON OIL YIELDS


Extraction With N-Hexane Extraction With Ethanol
S/N
Volume of Solvent used (ml) Mass of Oil % Oil Yield Mass of Oil % Oil Yield
Extracted (g) Extracted (g)

1. 100 7.623 38.12 6.003 30.02


2. 125 9.258 46.29 7.976 39.88
3. 150 10.040 50.39 8.324 41.62
4. 175 10.478 52.39 8.829 44.15
5. 200 10.527 52.64 9.159 45.80

B. PHYSICOCHEMICAL PROPERTIES
albidum seed oil. Since the free fatty acid of Pentaclethra
Table 4.1 presents the respective physicochemical properties macrophylla oil obtained is low, this suggest its usage as
of the extracted oil of Pentaclethra macrophylla benth. For the
physical properties, the oil extracted is raw sienne (dark edible oil. Also the acid value results shows 5.84mg/KOH/g)
brown) with ethanol and raw umber(light brown) with and 6.40mg/KOH/g) respectively for ethanol and n- hexane
n-hexane. The result is consistence with the one reported by extract respectively. This result is comparable to the
[5] and [6]). The refractive index for n-hexane and ethanol 7.350.12 and 7 acid value reported by [6].. The acid value is
extract of the oil are 1.466 and 1.453 respectively. The a measure of freshness and edibility of the oil. And for the
refractive index indicates the level of optical charity of the saponification value, the result indicates 152.72 and 164.39
crude oil sample in relative to water. The refractive index of respectively for ethanol and n-hexane extract. [5] and [10]
oil is a measure of how much a light ray is bent when if passes reported a saponification value of 158.403.40 and
from air into oil and is usually depends on the density of the 162.69mg/KOH/g respectively on some non conventional oil.
oil. This result was consistence to the 1.46 value obtained at The high saponification value recorded for the oil is an
25oC for oil bean by [7]; and 1.4672 obtained by [8] on indication that , the oil have potential for industrial used [12].
Chrysophyllum albidum seed oil. And these result show that,
the oil is not as thick as most drying oils whose refractive C. EFFECT OF PARTICLE SIZE ON OIL YIELD
indices fall between 1.475 and 1.485 [9]. Also the physical The results of effect of particle size on oil yield is shown in
analysis of the oil gave a pH of 6.10 and 7.14 respectively for table 4.2. The extraction was carried out using five different
ethanol extract and n- hexane. The result indicate that, the particle size of 0.85mm, 1.18mm, 2.36mm, 3.35mm and
ethanol extract is almost acidic in nature while n-hexane 6.70mm for both solvents. It was observed that as particle size
extract is almost neutral. The melting point for oil extract decreases ,oil yield increased for both solvents. The highest
were 48oC and 49oC respectively for ethanol and n-hexane. yield was noted when the particle size was 0.85mm with a
This values are higher than the 22oC1.02 reported by [6]. percentage yield of 42.06 and 32.51 respectively for
This results is an indication of the fluidity of the oil. The n-hexane and ethanol . Beyond this particle size , the oil yield
viscosity of the oil extract shows 0.9100cP and 0.9113cP decreases for both solvent as shown in figure 4.1. In addition,
respectively for ethanol and n-hexane. This low value of n- hexane extract a little more of the oil than ethanol in all
viscosity of the oil shows that , the oil has low resistant to cases of particle size used for this experiment.
shear force(stress). The density obtained for the oil were
0.918g/cm3 and 0.921g/cm3for ethanol extract and n- hexane
extract respectively. These results is an indication that the oil
is less dense than water and the result is comparable to 0.9111
value obtained by [10] on fluted pumpkin oil.
And for the chemical analysis, the results shows that the oil
obtained has low iodine value of 53.19mg iodine/100g of
sample and 76.4mg iodine/100g of sample for ethanol and
n-hexane respectively. Since iodine value of the Pentaclethra
macrophylla benth oil is lower than 100, it can be classified as
a non-drying oil. This means that, the oil has a low content of
unsaturated fatty acids. Iodine value is very important because
it help in the estimation of the individual fatty acid content of
the oil [11]. And because of the low value of the iodine value,
the oil cannot be used in varnish, coating and paint FIGURE 4.1: EFFECT OF PARTICLE SIZE ON OIL
industries. It could be suitable as lubricating oil and for soft YIELD
soap and candle production.
The free fatty acid obtained from the chemical analysis were The low oil yield experienced for larger (bigger) particle sizes
2.92 for ethanol extract and 3.20 for n-hexane extract. This is as a result of lesser surface area , thereby restricting the
values agrees with the 2.25 obtained by [8] on Chrysophyllum penetration of solvent into the core of the seed to leach the oil

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Comparative Extraction Of Some Non-Conventional Oil Seeds (Pentaclethra Macrophylla Benth) Using Different
Solvents

out of the seed. But the high yield experience in smaller


particles is attributed to the large surface area of the particles
which enable the solvent to penetrate into the core of the seed
to leach the oil out of the seed. Large particles have smaller
amount of surface areas and are more resistant to intrusions of
solvent and oil diffusion. Therefore , small amount of oil will
be carried from inside the large particles to the surrounding
solution.
D. EFFECTS OF TIME ON OIL YIELD
The extraction time is also called residence time or contact
time. This is very important in solvent extraction of oil
because it helps in choosing the most optimal time of
extraction. In this research work, extraction time of FIGURE 4.2: EFFECTS OF TIME ON OIL YIELD
20,30,40,50,and 60 minutes was used. The result is shown in
table 4.3 and also presented in figure 4.2.

STATISTICAL ANALYSIS:

IV. EFFECTS OF PARTICLE SIZE ON OIL YIELDS


SUMMARY OUTPUT FOR EXTRACTION WITH N-HEXANE

Regression Statistics
Multiple R 0.959
R Square 0.919681
Adjusted R Square 0.892908
Standard Error 2.520832
Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 218.2865 218.2865 34.35098 0.009904
Residual 3 19.06378 6.354594
Total 4 237.3503

Coefficients Standard t Stat P-value Lower 95% Upper


Error 95%
Intercept 42.21959 1.915663 22.03916 0.000204 36.1231 48.31609
Particle Size (mm) -3.14321 0.536295 -5.86097 0.009904 -4.84994 -1.43648

RESIDUAL OUTPUT

Observation Predicted Extraction Residuals


With N-Hexane (%
Oil Yield)
1 39.54786 2.512136
2 38.5106 0.489396
3 34.80162 -3.05162
4 31.68984 -1.23984
5 21.16008 1.28992

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International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-9, September 2014

SUMMARY OUTPUT EXTRACTION WITH ETHANOL

Regression Statistics
Multiple R 0.991443
R Square 0.98296
Adjusted R Square 0.977279
Standard Error 0.77186
Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 103.0988 103.0988 173.052 0.000949
Residual 3 1.787303 0.595768
Total 4 104.8861

Coefficients Standard t Stat P-value Lower 95% Upper


Error 95%
Intercept 33.36056 0.586562 56.87477 1.2E-05 31.49385 35.22726
Particle Size (mm) -2.16016 0.16421 -13.1549 0.000949 -2.68275 -1.63758

RESIDUAL OUTPUT

Observation Predicted Residuals


Extraction With
Ethanol (% Oil
Yield)
1 31.52442 0.985585
2 30.81156 -0.28156
3 28.26257 -0.71257
4 26.124 -0.334
5 18.88745 0.342547

2: EFFECTS OF TIME ON OIL YIELDS


SUMMARY OUTPUT FOR EXTRACTION WITH N-HEXANE

Regression Statistics
Multiple R 0.838667
R Square 0.703363
Adjusted R Square 0.604484
Standard Error 2.249209

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Comparative Extraction Of Some Non-Conventional Oil Seeds (Pentaclethra Macrophylla Benth) Using Different
Solvents

Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 35.98609 35.98609 7.113361 0.075878
Residual 3 15.17683 5.058943
Total 4 51.16292

Coefficients Standard t Stat P-value Lower 95% Upper


Error 95%
Intercept 33.676 3.017631 11.15975 0.001542 24.07255 43.27945
Time (min.) 0.1897 0.071126 2.667088 0.075878 -0.03666 0.416055

RESIDUAL OUTPUT

Observation Predicted Extraction Residuals


With N-Hexane (% Oil
Yield)
1 37.47 -2.45
2 39.367 2.273
3 41.264 1.566
4 43.161 -0.151
5 45.058 -1.238

SUMMARY OUTPUT EXTRACTION WITH ETHANOL

Regression Statistics
Multiple R 0.971136
R Square 0.943106
Adjusted R Square 0.924141
Standard Error 1.668599
Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 138.4584 138.4584 49.72963 0.005861
Residual 3 8.35267 2.784223
Total 4 146.8111

Coefficients Standard t Stat P-value Lower 95% Upper


Error 95%
Intercept 21.588 2.238661 9.643265 0.002367 14.46358 28.71242
Time (min.) 0.3721 0.052766 7.051924 0.005861 0.204176 0.540024

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International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-9, September 2014

RESIDUAL OUTPUT

Observation Predicted Extraction Residuals


With Ethanol (% Oil
Yield)
1 29.03 0.53
2 32.751 0.559
3 36.472 -2.502
4 40.193 1.207
5 43.914 0.206

3: EFFECTS OF VOLUME OF SOLVENT ON OIL YIELDS


SUMMARY OUTPUT FOR EXTRACTION WITH N-HEXANE

Regression Statistics
Multiple R 0.916377
R Square 0.839748
Adjusted R Square 0.78633
Standard Error 2.802651
Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 123.482 123.482 15.72047 0.028661
Residual 3 23.56456 7.854853
Total 4 147.0465

Coefficients Standard t Stat P-value Lower 95% Upper


Error 95%
Intercept 26.882 5.463373 4.920404 0.016084 9.495109 44.26889
Volume of solvent used 0.14056 0.035451 3.964904 0.028661 0.027739 0.253381
(ml)

RESIDUAL OUTPUT

Observation Predicted Extraction Residuals


With N-Hexane (%
Oil Yield)
1 40.938 -2.818
2 44.452 1.838
3 47.966 2.424
4 51.48 0.91
5 54.994 -2.354

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Comparative Extraction Of Some Non-Conventional Oil Seeds (Pentaclethra Macrophylla Benth) Using Different
Solvents

SUMMARY OUTPUT EXTRACTION WITH ETHANOL

Regression Statistics
Multiple R 0.917003
R Square 0.840894
Adjusted R Square 0.787859
Standard Error 2.845501
Observations 5

ANOVA
Df SS MS F Significance F
Regression 1 128.3789 128.3789 15.85536 0.028343
Residual 3 24.29063 8.096877
Total 4 152.6695

Standard Upper
Coefficients Error t Stat P-value Lower 95% 95%
Intercept 18.796 5.546903 3.388558 0.04282 1.143279 36.44872
Volume of solvent used
(ml) 0.14332 0.035993 3.981879 0.028343 0.028774 0.257866

using 1.18mm particle size of sample for 20 minutes each


with the following volumes- 100, 125, 150, 175 and 200 ml.
From the result, it was found that oil yield increased as the
volume of solvent increased from 100- 200ml.

Oil yield increased as the extraction time increased for


n-hexane and ethanol. The oil yield were seen increasing in
the first 20 minutes of extraction and thereafter the yield of oil
started reducing. As time increases from 20 to 60 minutes, oil
yield increases from 35.02% to 43.82% and from 29.56% to
42.12% respectively for n-hexane and ethanol. The highest oil Figure 4.3: EFFECTS OF SOLVENT VOLUME ON
yield recorded was at 60 minutes, though values were almost OIL YIELD
insignificant. The initial high rate of extraction may be due to the oil yield increases with volume of solvent up to 150ml,
quick solubility of the oil present at the solid surface and then the yield becomes less and insignificant as extraction
higher mass transfer driving force provided by low oil progresses. This was been reported by [9] in his studied of
concentration in fresh solvent. The later slower rate may be kinetics and thermodynamics study of oil extraction from
attributed to lower driving force due to increasing oil fluted pumpkin seed. Also [11] reported that, the positive
concentration in the solvent . effect of volume of solvent on oil yield was as a result of
increase in the concentration driving force as volume of
4.5: EFFECTS OF VOLUME OF SOLVENT ON OIL solvent increases. It was as a result of increased washing of oil
YIELDS extracted away from the particle surface by the solvent as a
result of increased volume. The highest percentage of oil
The effects of volume of solvent on oil yield is shown in table yield were attained when a solvent volume of 200ml was used.
4.4 and also in figure 4.3. The experiment was carried out But this was insignificant compare to when 150ml was used.

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International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-9, September 2014
V. CONCLUSION

It can be concluded that ethanol, a green and safe solvent is a


good replacement for n-hexane statistically. There is no
significant difference in the extraction efficiencies of
n-hexane and ethanol based on experimental parameters such
as time, volume of solvent and particle size affect the oil yield.
The oil properties reveal that the types of solvent has
influence over the oil properties with variance. Different
solvents will yield different extracts and extract compositions.
Finally, non-conventional oil seeds such Pentaclethra
macrophylla benth has great potential for oil that could
replace the conventional oil seeds industrially for the
production of soaps, candles, shampoo and the oil can be
regarded as edible.

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