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Renato O. Arazo, Michael R. Abonitalla, John Michael O. Gomez,

Nathaniel E. Quimada, Kyle Michael D. Yamuta, and Dennis A. Mugot, Philippines
Muhammad Usman Hanif, Pakistan


Extraction of oil from the seeds of Swietenia macrophylla was carried out to deter-
mine its potential for bio-oil production and the eventual making of liquid biodiesel products.
Central composite design of the response surface methodology was the experimental design
employed considering reaction time, catalyst loading and amount of methanol as operating
variables in the production of biodiesel. The biodiesel production, produced via transesteri-

and methanol. Hexane was used as the solvent in the extraction of oil from the seed. Essential
characteristics of the seed, the extracted oil from the seed, and the produced biodiesel were all
determined. The result showed that the seed has a moisture content of 10.6%. About 48.44%

biodiesels high heating value of 39.87 MJ/kg, generally equal to 40 MJ/kg of the commercial
heavy fuel. This work demonstrated that seeds from S. macrophylla are useful biomass in the

macrophylla seed

1.0 Introduction

The imminent depletion of oil from food-based products such as bioetha-

reserves around the world is becoming nol from corn, wheat or sugar beets sources
a major problem facing a world hungry -
for energy. Already, the high dependence ers have been commercially produced in
on the energy of the transportation sector
creates a volatile market with ever increasing ever, the debate of food security versus bio-
prices of petroleum-derived fuels (Jacobson, fuel production continues to be a challenge
Maheria, Dalai, & Kumar Dalai, 2013). This
havoc prompts many concerned individu- generation biofuel sources. Second genera-
tion biofuel from lignocellulosic feedstocks
could substitute the need for fuel, particu- (like agricultural wastes), non-food crops
larly liquid fuel, needed for transportation. and forest products are likewise used in
The abundance of biomass worldwide is
seen as one promising alternative source Swietenia macrophylla is one of the
of energy. Exploitation of various biomass tropical trees that could potentially provide
sources has been explored in the produc- biofuel products. Among the less utilized
tion of biofuels. First generation biofuels parts during fruiting stage are the matured

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discarded. Particularly, more than 50% of where MC is the moisture content of the
the components of the seed of the S. mac- seeds, Mi is the initial mass of the seeds and
rophylla are carbon (48.14%) and hydrogen Mf is the mass of the seeds after oven dry-
(6.4%), the elements composing the biofuel ing.
products (Kader, Joardder, Islam, Das, &
Hasan, 2012). With appropriate extraction 2.2 Oil Extraction from S. macrophylla
method, compounds comprising carbon and Seeds
hydrogen present in the seeds could become
the elemental composition of a biofuel Oil extraction adopted the methods
product either solid biochar, liquid bio-oil, reported elsewhere in extracting oils from
or biogas. seeds (Liauw et al., 2008). Sundried seeds
Among the biofuels that needs in- were pulverized manually using mortar and
tensive research considering its infancy pestle. For 24 h, the 25 g of ground seeds
stage is the production of liquid biofuel in were soaked in 40 mL n-hexane in the closed
the form of bioethanol, bio-oil, biogasoline 100 mL beaker. After 24 h, the mixture was
and biodiesel. In this work, the oil of the S. -
macrophylla seeds was extracted and pro-
cessed with the ultimate goal of producing plate at 60 o
high-quality biodiesel. Response surface was allowed to cool and weighed to con-
methodology was employed to carefully stitute the extracted oil. The oil yield was
study the interactive and overlapping ef- calculated using Eq 3.
fects of all the operating variables and got
the best conditions that would optimize bio-
diesel production.

2.0 Materials and Methods where %Y is the percent yield of the oil
extracted, m is the initial mass of the S.
2.1 Preparation of S. Macrophylla Seeds macrophylla seed, and m is the mass of the
extracted oil.
The S. macrophylla capsules were
collected from Claveria, Misamis Oriental, 2.3 Experimental Design of Biodiesel Pro-
Philippines. The seeds were manually tak- duction
en from the capsules and sundried in 10 h
(Aliyu, Lomsahaka, & Hamza, 2012). The The Central Composite Design
moisture content of the sundried seeds was (CCD) of the Response Surface Method-
calculated following ASTM E1756, and us- ology using Design Expert 7.0 software
ing Eqs 1&2. was employed as the statistical tool of the
study. Response surface methodology
(RSM) consists of a group of mathematical
and statistical techniques used in the devel-
opment of an adequate functional relation-
ship between a response of interest, y, and
some associated control (or input) variables
denoted by x1,x2, ... ,xk (Gunst, 1996).

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The main objective of RSM is to deter- to the nominal target requirements, and re-
mine the optimum operational conditions duced development time and overall costs.
of the system or to determine a region that The CCD was initializing how
many grams of potassium hydroxide and
application of statistical
experimental methanol are to be added, and how long it
- would be stirred in the reaction container.
cess development can result in improved The ranges and levels of operating variables
product yields, reduced process variability, used in the experiment of biodiesel produc-
tion were given in Table 1.
Table 1. Experimental Range and Levels of Independent Variables

With the values of independent vari- The effect of the amount of potassi-
ables in Table 1, there were 20 runs generat- um hydroxide and methanol, and the reac-
ed and was conducted for experimentation. tion time to biodiesel yield was determined
and analyzed via 3D models generated
2.4 Biodiesel Production through Transes- using RSM. Analyses include the deter-

Variance (ANOVA), diagnostics and 3D

The laboratory grade potassium model graphs generation.
hydroxide and methanol were all purchased Numerical optimization was con-
from Harnwell Marketing, Cagayan de ducted to determine the Design Expert soft-
Oro City, Philippines. Potassium hydrox- wares suggested solutions for the best con-
ide (KOH), used as a catalyst, is in pellet ditions to have optimum yield of biodiesel.
Solutions with high desirability were tested
as KOH while methanol has 99.8% purity.
About 20 mL of extracted seed oil was -
mixed to appropriate amount of methanol tive to the predicted/theoretical value was
and KOH into the beaker. The mixture was considered as the best condition to achieve
heated and continuously stirred at 65 oC in optimum biodiesel yield.
a hot plate at predetermined reaction time.
After 24 hours cooling, the glycerin and 2.6 Product Analysis
the biodiesel were separated by decanta-
Percent yields of produced biodiesel
an ambient atmosphere for 30 min to allow were determined using analytical balance.
excess alcohol to escape from the product The pH values of the yields were deter-
through volatilization. mined using the pH meter. The densities of
the yields were computed using the standard
2.5 Modeling and Optimization
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ratio of mass and volume of a given sample. functional groups found in the product yields.
Bomb Calorimeter following ASTM D4809 The experimental set-ups of oil
determined the high heating value (HHV)
process are illustrated in Figures 1 and 2.

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3.0 Results and Discussion 2. The highest and least moisture contents
of the seeds were recorded at 10.30% to
3.1 Moisture Content of S. macrophylla 11.0%, respectively. The moisture content
Seeds of S. macrophylla is somehow closer to the
results of some studies in biodiesel produc-
The moisture content of the S. tion using Jatropha curcas L seed oil which
macrophylla seeds after drying was deter- is between 7.4%10.7% (Moulana, Satri-
mined in three (3) trials as shown in Table ana, Supardan, & Aina, 2013).

The presence of moisture content diesel production (Joseph, Chidozie,

in seeds helped the reaction both the polar Obioma, Christopher, & Emeka, 2014).
and non-polar compounds. The polar com-
pounds which were not good in biodiesel 3.2 Percentage Yield of Oil Extracted from
production remained in the water while the S. macrophylla Seeds
nonpolar compounds of the S. macrophyl-
la seeds reacted the methanol which is also The seed of S. macrophylla gave
- crude oil yield of 30.36%48.44% by mass
tion occurred. High moisture content in the
seeds affected the amount of free fatty acids of previous studies with oil yield from S.
- macrophylla seed between 33%53% using
tion process. High water levels caused hy- boiling and skimming extraction method
drolysis, fatty acids in biodiesel is converted (Aliyu et al., 2012; Kim, 2013).
into free fatty acids, thereby increasing the
acid number that can corrode engine parts
and injection system (Vicente, Martnez, &
Aracil, 2004). Other study reported max-
imum oil recovery at 6% moisture content
and found that the increased of the moisture
content to 14% resulted in a decrease in the
oil recovery by 16% (Olayanju, Akinoso,
& Oresanya, 2006). Besides, the water in
the seed may be elevated to the liquid oil
product during extraction which caused
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The high percentage of oil that can The density and pH of bio-oil from
be extracted from S. macrophylla seed us- S. macrophylla seed were determined (Ta-
ble 3). The density of the bio-oil from S.
the same literature (Vicente et al., 2004). macrophylla seed is 0.862 g/cm3 which
The n-hexane is widely used solvent in oil
extraction because of its ideal functionality use (Valente, Pasa, Belchior, & Sodre,
for maximum extraction (Swanson, 2009). 2011). The relative density of the oil from
It is nonpolar and apparently dissolved non- S. macrophylla was found to be within the
polar compounds in the seeds following the limits of biodiesel fuel standard (Joseph et
chemistry rule that like dissolves like. It al., 2014). The lower the density, the heavi-
means nonpolar compounds in the seeds er the fuel and the harder it is to burn. Con-
were dissolved by n-hexane and became versely, the higher density, the lighter the
fuel and the poorer the fuel mileage (Janka,
were separated. 2000).

3.3 Properties of S. macrophylla Seed Oil

The pH level of extracted oil is ic bio-oils are corrosive to common metals

6.250.83 which is nearly neutral, a desir- such as carbon steel and aluminum, and it
able result considering that this would not can affect the engine, especially with ele-
trigger corrosion problem in pipelines and vated temperature and with the increase in
vessels of engines (Arazo, 2014). The acid- water content (Yu et al., 2007).
Table 4. Percentage Yield of the Biodiesel from S. macrophylla Seed Extract

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The yield of biodiesel from S. mac- et al., 2012). This result is also much higher
rophylla compared to the previous study of extract-
process ranges from 36.10%84.30% (Table ing oil from S. macrophylla seed with 53%
recovery (Aliyu et al., 2012).
J. curcas seed oil, the widely used non-ed-
ible biodiesel feedstock with extracted oil 3.5 Effects of the Chosen Parameters to the
content from 30% to 50% by weight (Aliyu Yield of the Biodiesel

Figure 4. 3D Response Surface on the Yield of Oil Extracted from

S. macrophylla Seeds

Figure 4 shows the effect of potas- The quadratic model equation gen-
sium hydroxide and methanol on the yield erated by CCD using the Design Expert 7.0
of biodiesel from S. macrophylla seed oil. -
dict the biodiesel percentage yield (Eq 4).
resulted in a substantial decrease of bio-
diesel yield. On the other hand, the increase
of methanol led to an increase in the yield
of the biodiesel. Increasing the amount of
alcohol at minimum catalyst in the trans- where %Yield is the predicted percent-
age yield of biodiesel, KOH that was used
to the increase of yield (Khurshid, 2014). during the extraction process, B is the meth-
anol that was added during the reaction, and
C is the reaction time.
macrophylla Seed Oil

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Table 5. ANOVA of the Yield of Biodiesel from S. macrophylla

Based on the predicted model, ables, to improve the accuracy of the model.
there is an expected decrease in the bio- Overall, the result implied that the yield of
diesel yield when the amount of KOH is the biodiesel from seed extracts could be
increased. The biodiesel yield can also be appropriately modeled with high reliability.
reduced with the interactive effect of AB
(KOH and methanol), and quadratic values 3.7 Properties of the Produced Biodiesel
of B (methanol) and C (reaction time). This
result is further supported by the result of The functional groups present in
the analysis of variance (ANOVA) shown in the biodiesel extracted from the S. macro-
Table 5. The p-value of 0.0031 implies that phylla -
the model has only 0.31% chance of com- ysis in the wavelength between 9523989
mitting an error in predicting the percent- cm-1 wave numbers (Figure 5). The possi-
age yield of biodiesel. This outcome means
that there is an assurance of 99.69% that the functional groups were tabulated in Table 6.
biodiesel can be correctly calculated using
Eq 4. The reliability of the model is further

model is well suited and can appropriately

estimate the yield of biodiesel from the S.
macrophylla seed extract.
The term A, AB and B2 and C2 are

cantly affect the yield of biodiesel from the
Figure 5. Fourier Transform Infrared Radi-
model terms greater than 0.05 were exclud- ation (FTIR) Spectrum of Biodiesel from S.
ed in the model except the independent vari- macrophylla Seed Extract

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A broad absorption band observed ing vibrations suggesting the presence of

between 35003000 cm-1 is attributed to ketones, aldehydes, and esters (Arazo,
the OH stretching of hydroxyl groups from 2014). The spectra at 10001300 cm-1 in-
phenols, alcohols, carboxylic groups and dicates the possible presence of esters in
NH stretching of amines and amide groups. the CO stretch group. The C=O stretching
The observed peak between 28503000 and OH bending group between 1300950
cm-1 is caused by CH stretch suggesting cm-1 indicated the presence of alcohols in
the presence of alkanes. The presence of the product. Another group of aromatic
C=C stretch in 14001600 cm-1 indicates compounds is possibly present considering
the presence of aromatic compounds. An- the band between 900675 cm-1 of the CH
other band observed between 16701820 stretch group (Arazo, 2014).
cm-1 are possibly caused by C=O stretch-

Table 6. The FTIR Functional Groups of Biodiesel from S. macrophylla Seed Extract

- 4.0 Conclusions
duced biodiesel resulted to 39.87 MJ/kg
high heating value which passes the 39.80 This work explored the potential
MJ/kg requirement of commercial biodies- of using the seeds of S. macrophylla in the
el products (Gerpen, Shanks, Pruszko, & production of biodiesel. The following are
Clements, 2004). This result means that the the major conclusions drawn from this in-
biodiesel from the S. macrophylla seed oil vestigation:
can be used commercially considering that 1. The S. macrophylla seeds, after
the product possessed the required energy sun drying, contains acceptable moisture
of a commercial biodiesel. Moreover, anal- content ready for oil extraction.
ysis result revealed 0.12% sulfur content of 2. The S. macrophylla seeds have
the product, a little higher value to the max- abundant oil that can be extracted with
imum limit of 0.05% (Strong, Erickson, & equivalent yield, density, and pH from those
Shukla, 2004). With employment of appro- of other seed-based crude oil from other
priate measures to further reduce the sulfur plants.
content of the product, the biodiesel from S. 3. The percent recovery of biodiesel
macrophylla seed is a very promising liquid from the S. macrophylla seed oil is much
fuel to substitute the petroleum-based die- higher compared to that of the widely used
sel. non-edible J. curcas seed oil.
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4. Response surface methodology Gunst, R. F. (1996). Response Surface

can model the biodiesel yield with high reli- Methodology: Process and Prod-
ability. Notably, the reduced quadratic mod- uct Optimization Using Designed
Experiments. Technometrics. 38(3).
from S. macrophylla seed oil and found sig- 284286. Retrieved from https://
5. The biodiesel from S. macrophyl-
la seeds indicated the presence of esters Jacobson, K. et al. (2013). Bio-oil valori-
(C0 stretch), alkanes (CH stretch), aro- zation: A review. Renewable Sus-
matic (C=C stretch) carbonyl (C=O stretch), tainable Energy Reviews, 23.
hydroxyls (OH stretch), and alcohol (C=O 91106.
6. The biodiesel product has the Janka, J. W. (2000). Properties of Diesel
needed energy to run engines with a high Fuel can Affect Performance.
heating value of 39.87 MJ/kg, a value high-
er than the 39.80 MJ/kg requirement of Joseph, C. O. et al. (2014). Potentials of
commercial biodiesel products. Non-edible Abrus precatorius Seed
7. A ton of S. macrophylla (mahoga- Oil Towards Biodiesel Production.
ny) seeds can produce 420 L bio-oil and 352 African Journal of Biotechnology,
L biodiesel. 13, 42264235. Retrived from
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