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Increased Bio-Oil Yield From Swietenia Macrophylla Seeds Via Microwave Pretreatment and Ultrasonic-Assisted Solvent Extraction
Increased Bio-Oil Yield From Swietenia Macrophylla Seeds Via Microwave Pretreatment and Ultrasonic-Assisted Solvent Extraction
Increased Bio-Oil Yield From Swietenia Macrophylla Seeds Via Microwave Pretreatment and Ultrasonic-Assisted Solvent Extraction
Rey P. Gumaling, Jay R.E. Agusan, Neil Ven Cent R. Ellacer, Gretel Mary T. Abi Abi,
Jasmin Roxatte P. Pajaron, Jose Rey Q. Joyno, Cherry Q. Joyno, Alexander L. Ido,
Renato O. Arazo
PII: S2468-2039(18)30103-1
DOI: 10.1016/j.serj.2018.06.003
Reference: SERJ 136
Please cite this article as: Gumaling RP, Agusan JRE, Cent R. Ellacer NV, Abi Abi GMT, Pajaron JRP,
Joyno JRQ, Joyno CQ, Ido AL, Arazo RO, Increased bio-oil yield from Swietenia macrophylla seeds
through microwave pretreatment and ultrasonic-assisted solvent extraction, Sustainable Environment
Research (2018), doi: 10.1016/j.serj.2018.06.003.
This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to
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pretreatment and ultrasonic-assisted solvent extraction
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Rey P. Gumaling a, Jay R E. Agusan a, Neil Ven Cent R. Ellacer a, Gretel Mary T.
Abi Abi a, Jasmin Roxatte P. Pajaron a, Jose Rey Q. Joyno a, Cherry Q. Joyno a,
Alexander L. Ido a, Renato O. Arazo a,b*
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a
College of Engineering and Technology, University of Science and Technology of
Southern Philippines, Claveria 9004, Philippines
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b
Project Development Office, University of Science and Technology of Southern
Philippines, Claveria 9004, Philippines
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*Corresponding author
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Abstract
Low recovery coupled with intensive energy requirement due to long processing
time makes the potential of bio-oil production not seamlessly appreciated. In this study,
the optimization of bio-oil yield from non-edible Swietenia macrophylla seeds through
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microwave pretreatment before ultrasonic-assisted solvent extraction was investigated.
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Central composite design of response surface methodology was employed to analyze the
effects to the bio-oil yield of the irradiation time (4-8 min) and irradiation power (90-450
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W) as pretreatment variables using a microwave oven at 2.45 GHz frequency. Results
showed that microwave pretreatment significantly increased the bio-oil yield by 5% with
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optimum recovery of 43% at shortened pretreatment time of 7 min instead of 6 h in the
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conventional oven heating method. The bio-oil yield increased when the irradiation time
was increased, while irradiation power showed no significant effect. Analysis of the
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similar functional groups present both in the extracted bio-oils from the microwave and
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the conventional pretreated seeds indicating that the former pretreatment, like the latter,
did not destruct the compounds present in the seeds. The study demonstrated that the
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seeds of S. macrophylla have strong potential for bio-oil production and poise huge
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1. Introduction
The finite source of petroleum oil reserve would be exhausted in the next century
due to the increasing consumption of crude oil products to feed engines [1]. The
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industrialization in the developed and developing countries, contributes greatly to the
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increased greenhouse gases in the atmosphere which cause the global climate change [2].
Hence, the twin crises of fossil fuel depletion and environmental degradation attract
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researchers to continually search for an alternative energy resource that is sustainably
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Interest in biofuels, like liquid biodiesel with bio-oil feedstock, is becoming more
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attractive due to its renewable origin and environmental benefit of emitting less carbon
dioxide, sulfur oxides and hydrocarbon [3]. More importantly, the bio-oil derived from
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second and third generation biomass like Swietenia macrophylla seeds [4], Hevea
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brasiliensis seeds [5], and microalgae [6] as feedstocks for biodiesel production were
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preferred over the first generation like corn, wheat, peanut, and coconut to avoid the
Related literature shows that bio-oil from S. macrophylla seeds contain common
unsaturated fatty acids such as oleic (26%), linoleic (33%), linolenic (12%) and saturated
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fatty acids, namely, palmitic (13%) and stearic (14%) suggesting its suitability for
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biodiesel production [7]. These fatty acids could be recovered through suitable extraction
method that would maximize bio-oil yield. One of these is the ultrasonic-assisted solvent
extraction (UASE) method that ruptures the membrane of the S. macrophylla seeds
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advantageous not only because of increase bio-oil recovery but also in the reduction of
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processing time needed as compared to conventional pretreatment [8,10–13].
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To date, there has been no study yet on the optimization of bio-oil yield from S.
macrophylla seeds when subjected to microwave pretreatment (MWP). In this work, the
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seeds of S. macrophylla, an oil-rich second-generation biomass from an exotic Philippine
species of the family Meliaceae, were used to produce bio-oil, a potential feedstock for
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biodiesel production [4,14]. It ultimately aims to give scientific information on the effects
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of MPV to the bio-oil recovery from S. macrophylla seeds. Specifically, optimization of
the bio-oil yield was investigated considering the effects of irradiation time and
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irradiation power as operating variables through the central composite design (CCD) of
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response surface methodology. This is an appropriate statistical tool that does not only
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serve for the design of experiments but also capable of giving 3D plots to closely
investigate the effects and determine the optimum values of chosen variables [15]. The
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functional groups present in the produced bio-oils were, likewise, identified through
The S. macrophylla seeds used in this study were collected from Poblacion,
Claveria, Misamis Oriental, Philippines. The pods were broken to collect the seeds. The
whole seeds were sundried, cleaned by airing, oven dried (Contherm Designer Series
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before pretreatment and extraction. Only those particles that passed the sieve were used
as biomass.
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2.2 Parametric and optimization studies
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according to the literature [10,11] such as irradiation time and irradiation power. The runs
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were based on the parametric study principle of taking one variable as constant while
varying other variable, and a peak was known in a graph once plotted. The values of the
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observed peaks were used as center points (level 0) of the variables.
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Based on the parametric investigation of this work, the levels and range of values
of the variables were known (Table 1) and were used in the design of experiment in the
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In the optimization study, the CCD of response surface methodology was used in
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the design of experiment with the aid of Design Expert 7.0 software. The combinations of
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all runs, consisting irradiation time and power, were based on experimental design
generated by the CCD. The experiment was conducted at room temperature (25 ± 1 °C).
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For each run, 15 g of oven dried powder of S. macrophylla seeds were placed in the plate
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of a microwave oven (JEI2340WPSL GE Model, China) with 2.45 GHz frequency and
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following the predetermined irradiation time and power. After which, the pretreated
samples were cooled down inside the desiccator. Fig. 1 describes the pretreatment
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Pretreated powdered seeds were subjected to UASE using n-hexane following the
experimental procedures described in the study of Mabayo et al. [5]. The n-hexane (96%,
GR grade, Duksan Pure Chemicals) used in the bio-oil extraction was purchased from
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Harnwell Chemical, Cagayan de Oro City, Philippines. The experiment was conducted at
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the Chemistry Laboratory of the University of Science and Technology of Southern
Philippines with a room temperature of 25 ± 1 °C. Each UASE run, with variable
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irradiation time and power set according to the design of experiments, was done with 75
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sonication time, and 15 g powdered seeds.
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2.4 Control set-up for MWP
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To compare the results that were generated from the optimization study and to
determine the efficiency of MWP, a conventional heating using the oven as control
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experiment was conducted. For the control experiment, powdered S. macrophylla seeds
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for 6 h [11].
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The percent bio-oil yield from S. macrophylla seeds was determined using digital
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analytical balance. The percent yield was calculated using Eq. (1).
% 100 (1)
where %Y is the percent yield (wt%) of the bio-oil extracted from powdered seeds, m1 is
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the mass of produced bio-oil, and m2 is the mass of powdered seeds used in extraction.
Proximate analyses of the powdered seeds in terms of moisture content and ash
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content from microwave heating and conventional oven heating were conducted and
analyzed. The moisture content was determined using drying oven (Contherm Designer
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Series Oven, Model: CE Z011) at 100 ± 1 °C for 24 h. The LabTech LEF-304P-2 muffle
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furnace was used in ash content analysis at 600 ± 25 °C for 3 h.
The bio-oils, both from microwave and conventionally pretreated seeds, were
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subjected to FTIR spectroscopy analysis to compare if there are differences in the
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functional groups. The FTIR spectroscopy analysis was conducted at the Pilipinas Kao,
Statistical analysis and modeling were done through CCD using Design Expert
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7.0 software. Analysis of variance was the statistical tool used in the study that
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determined the most appropriate model equation that best fits the data gathered in the
experimental runs. The percent yield of the experimental runs underwent graphical
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modeling and established the interactive effects of the chosen operating variables through
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and physical appearance were determined before these were utilized as feedstock. The S.
macrophylla fruit pod was brown with oval seed (Fig. 2). Each winged pod weighed 0.2
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± 0.1 g while each seed weighed 0.5 ± 0.1 g. The seeds moisture content recorded 6.1 ±
0.2%, on wet basis, which is lower than the 10.6 ± 0.4% reported elsewhere [4]. Low
moisture content is desirable considering the least possibility that water shall be elevated
to the liquid product during bio-oil extraction. The recorded S. macrophylla seed’s ash
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content of 10.9±0.1% is just comparable to diverse bio-based fuel products [16]. As a
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supplementary data from other work, the ultimate analysis of S. macrophylla seeds
showed that the carbon, hydrogen, nitrogen, sulfur, and oxygen percent contents were
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48.14, 6.40, 0.28, 0.03, and 45.15, respectively [17].
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3.2 MWP parametric analysis
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Fig. 3a shows the bio-oil yield from 15 g microwave pretreated S. macrophylla
seeds produced at variable irradiation powers with 3 min irradiation time. The bio-oil
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yield peaks at 270 W irradiation power (42.4%). This result was used as the center point
(level 0) in making the level and range of MVP variable in this study (as shown in Table
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1).
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At 270 W irradiation power as constant and variable irradiation times, the bio-oil
yield peaks at 6 min with 43.5% yield (Fig. 3b). The design of experiment used the 6 min
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as the center value (level 0) of the irradiation time (as shown in Table 1).
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Therefore, the 270 W irradiation power and 6 min irradiation time were taken as
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the center of the levels of variables in the design of experiment of independent variables
As seen in Table 2, the highest bio-oil yield of 46 wt% was achieved at 8 min
irradiation time and 270 W irradiation power; while the lowest yield of 39 wt% was
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achieved at 5 min irradiation time and 180 W irradiation power. This means that the large
increase in irradiation time and a small increase in irradiation power during pretreatment
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3.4 Model fitting of bio-oil yield as subjected to MWP
The CCD’s analysis particularly the fit summary revealed that response surface
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quadratic model best fitted in predicting the percentage of bio-oil yield from S.
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macrophylla seeds as affected by MWP variables. The ANOVA result of the response
surface quadratic model for the percentage of bio-oil yield is shown in Table 3.
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The model p-value of 0.0001 indicates a highly significant quadratic model with
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high accuracy in predicting the bio-oil yield of microwave pretreated S. macrophylla
seeds. The model p-value of 0.0001 means that there is only 0.01% chance that error
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could arise from the noise. The lack of fit F-value of 0.35 implies that the lack of fit is not
significant relative to pure error and that there is 79.1% chance that the lack of fit F-value
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this large could arise through the noise. It is good to note that the lack of fit is not
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The coefficient of variance and determination could also support that the
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quadratic model is robust. The coefficient of determination (R2) value of 0.96 is high
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which means that the regression model for the bio-oil yield was satisfactory and
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demonstrated a high degree of correlations between the actual data and predicted values.
It also signifies that there is 96% certainty that the generated model can explain the
variability of the data. Further, the adjusted coefficient of determination (Adj. R2) of 0.93
is also high which could support the suitability of generated model in presenting the
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1.15% was low enough to represent adequacy of data indicating that the model owns high
precision and reliability for fitting experimental values. Eq. (2) shows the quadratic
model equation in terms of actual factors where A and B represent irradiation time (min),
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37.71 − 1.76 + 0.03 − 0.01 + 0.44 (2)
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The predicted values of bio-oil yield could be determined using the generated
quadratic equation. This equation could also support how the terms affect the bio-oil
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yield. Unlike term B (irradiation power), term A (irradiation time) was found significant
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and has a negative numerical coefficient which means that increasing the irradiation time,
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when taken singly, may lead to a decrease in yield, but the square of it (A2) resulted
otherwise. Hence, the model equation can be further investigated using a 3D plot to
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determine the overall effect of the two contrasting coefficients of A and A2 terms. The
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overall result showed that the effect of irradiation time (A and A2 combined) significantly
Table 4 shows that the actual values were seen close to the predicted values which
could further support the claim that the model fitness owns high degree of correlations
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between the actual and the predicted ones. Fig. 5 shows the diagnostic graph of the actual
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versus predicted responses of the experimental runs. The actual values according to data
points on the graph are positioned close to the predicted values represented by the straight
line signifying a high degree of correlations between the actual and predicted values (Fig.
5). This could mean that the model fitness is strong and reliable. This result supports the
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claim that response surface quadratic model is the most suitable model for predicting the
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Fig. 4 illustrates that as the irradiation time increases, the bio-oil yield increases.
A similar finding was observed by others [10,12,18,19]. This result clearly shows that
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increasing the exposure time could provide greater rupture of cell structure. Irradiation
power, on the other hand, has no statistical basis to support its significant effect on the
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bio-oil yield. Nonetheless, the Fig. 4 illustrates that the increase of irradiation power at
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the shorter time resulted in little addition of the bio-oil yield. At longer irradiation time,
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the increase of irradiation power resulted in a small and insignificant increase of bio-oil
product. This result implies that irradiation power effect is not significant when compared
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to irradiation time.
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Numerical optimization suggested two solutions that could result in optimum bio-
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oil yield from S. macrophylla seeds via MWP. The solution with the highest desirability
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was chosen and ran in triplicate following the suggested values of the operating variables.
The validated or the actual bio-oil yield of 43.3 ± 0.3% is close to the theoretical yield of
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43.8% with the percent error of 0.8–1.8% (7 min at 180 W). The percent error falls below
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the 5% acceptable error signifying that the model is valid and owns high degree of
precision in predicting the bio-oil yield from S. macrophylla seeds. This outcome means
that the bio-oil yield of the microwave pretreated seeds can be determined using the
equation generated by simply plugging in the values of irradiation time and power.
Ping et al. [8] reported the bio-oil yield of 29.5 ± 1.6% from S. macrophylla seeds
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applying MWP followed by solvent extraction using the mixture of methanol and
chloroform. The optimum condition in this study applying the same pretreatment
technique followed by ultrasonic-aided hexane extraction was way higher than the
reported yield in the study of Ping et al. [8]. This finding implies that the CCD of
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response surface methodology helped in making result way higher than the previously
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reported bio-oil yield as well as in establishing the optimum conditions. Further, the
finding tells that the use of hexane as a solvent in the ultrasonication could significantly
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increase the bio-oil yield from S. macrophylla seeds.
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3.7 Comparison of MWP with the conventional method
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To identify the best pretreatment method, conventional oven treatment of the
seeds was compared with MWP under the optimal conditions. MWP under 180 W power
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at 7 min time enabled to extract 43.3 ± 0.4%, which is apparently superior to that of
conventional treatment with 37.9 ± 0.1% yield under 60 °C temperature and 6 h time.
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This result means that MWP could promote the UASE of bio-oil. The result is also true
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with the study of Ren et al. [11] wherein MWP could enhance bio-oil extraction from
flaxseeds. The high extraction yield of microwave pretreated S. macrophylla seeds could
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The moisture and ash contents of pretreated S. macrophylla seeds were analyzed.
Its powder’s moisture content on dry basis of 4.8 ± 0.1% could be reduced to 3.4 ± 0.1%
through microwave treatment method. This result could be due to the quick and efficient
release of moisture when the seeds were subjected to MWP. It was also observed in the
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study of Wang et al. [20] wherein the biomass became dehydrated after being subjected
to microwave heating. Likewise, ash content could be reduced from 10.8 ± 0.02% to 9.1
± 0.4% using MWP. This outcome could be due to the ability of microwave heating to
modify the cellular structure causing lower organic compound content in the S.
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macrophylla seeds [20]. The less moisture and ash contents in S. macrophylla seeds are
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desirable because it can solve ignition and combustion problems when used as feed in
engines [16]. Further, the low moisture and ash contents are good considering the less
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possibility that water and ash will be elevated to the products during extraction stage.
The extracted bio-oil from microwave pretreated and conventionally treated seeds
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were subjected to FTIR analysis to determine whether they both possess the same
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functional group or not. The spectral features of bio-oil from S. macrophylla seeds are
displayed in Fig. 6.
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The actual peaks of the extracted bio-oils were identified, and the corresponding
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functional groups were determined. The absorption peaks at 3008.0 cm-1[a] and 3001.2
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cm-1[b] are due to C-H asymmetric stretch suggesting the presence of alkene. Peaks
appearing at 2918.7 cm-1[a] and 2916.8 cm-1[b] are due to the C-H symmetric of alkyl
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compounds, while, 2847.3 cm-1[a] and 2840.6 cm-1[b] are due to C-H antisymmetric stretch
alkyl group from lipids. The absorption peaks at 1743.7 cm-1[a] and 1733.3 cm-1[b] are due
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to C=O stretch indicating the possible presence of ester carbonyl group. Peaks appearing
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at 1465.1 cm-1[a] and 1461.2 cm-1[b] are assigned to the C-H antisymmetric deformation
vibrations suggesting the presence of methyl esters while 1375.2 cm-1[a] and 1374.1 cm-1[b]
peaks are assigned to the symmetric deformation vibrations, respectively. The bands at
1231.3 cm-1[a], 1227.2 cm-1[b], 1161.5 cm-1[a], and 1161.2 cm-1[b] correspond to the C-O
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stretching vibration suggesting the possible presence of the ester groups. The peaks at
722.1 cm-1[a] and 723.7 cm-1[b] are due to C-H bond from long-chain alkane. All identified
compounds present in the S. macrophylla bio-oil are also reported by others [14,21–23].
The results showed similar functional groups present in the extracted bio-oils from the
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conventional oven pretreated, and microwave pretreated seeds indicating that the
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compounds before extraction were not destructed to both MWP and conventional
pretreated processes.
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4. Conclusions
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In this study, the optimization of bio-oil yield from non-edible S. macrophylla
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seeds through MWP before UASE was investigated. MWP of S. macrophylla seeds
before UASE proved to increase the bio-oil yield by 5% with optimum recovery of 43.3 ±
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0.3 wt% at 180 W irradiation power and 7 min irradiation time. Increased in irradiation
time, during the MWP of S. macrophylla seeds before extraction process, significantly
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increased the bio-oil yield; while irradiation power has no statistical basis to support its
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significant effect on the bio-oil yield. Characterization of the bio-oil product through
FTIR spectroscopy showed similar functional groups both in the microwave and
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conventionally pretreated seeds suggesting the presence of alkanes, alkenes, esters, and
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other alkyl and carbonyl groups indicating the presence of desirable compounds for the
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production of biodiesel fuel and bringing into the center stage the huge implications of
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Acknowledgment
The authors would like to acknowledge the faculty and staff of the College of
Philippines in Claveria, Philippines, for the support in the conduct of the study.
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Coded level
Variable
−2 −1 0 1 2
Irradiation time (min) 4 5 6 7 8
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Irradiation power (W) 90 180 270 360 450
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3 6 270 40.7
4 6 270 42.0
5 6 450 42.5
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6 6 270 41.3
7 5 360 40.9
8 6 270 40.9
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9 8 270 45.8
10 6 90 41.9
11 6 270 40.5
12 7 360 43.3
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13 4 270 39.8
UASE: 15 g powdered seeds, 15 min sonication time, 75 mL hexane, 50 µm resonance amplitude, 60 ± 5
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°C temperature
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Table 3. ANOVA of the model for percentage bio-oil yield as influenced by MWP
Source Sum of df Mean F p-value
squares square value Prob > F
Model 37.5 5 7.50 32.4 0.0001a
A− Time 30.4 1 30.4 131 < 0.0001a
B− Power 0.159 b
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0.58 1 0.58 2.48
AB 1.58 1 1.58 6.80 0.035a
A2 4.35 1 4.35 18.8 0.003a
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B 1.73 1 1.73 7.46 0.029a
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Residual 1.62 7 0.23
Lack of fit 0.34 3 0.11 0.35 0.791b
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Pure error 1.28 4 0.32
Cor total 39.1 12
2 2
R = 0.96 Adj. R = 0.93 C.V.% = 1.15
Std. dev. = 0.48 Mean = 41.7 Adeq. precision = 20.3
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a
significant; b insignificant
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2 7 180 43.8 43.8
3 6 270 40.7 41.1
4 6 270 42.0 41.1
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5 6 450 42.5 42.6
6 6 270 41.3 41.1
7 5 360 40.9 41.1
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8 6 270 40.9 41.1
9 8 270 45.8 46.0
10 6 90 41.9 41.7
11 6 270 40.5 41.1
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12 7 360 43.3 43.0
13 4 270 39.8 39.6
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UASE: 15 g powdered seeds, 15 min sonication time, 75 mL hexane, 50 µm resonance amplitude, 60 ± 5
°C temperature
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LEGEND AN
1 – Microwave reactor 5 – Support roller ring
2 – Control panel 6 – Turntable motor hub
3 – Turntable plate 7 – Microwave door
4 – S. macrophylla seeds powder
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in petri dish
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Whole seeds with pods Whole seeds without pods Seeds powder
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Fig. 2. The S. macrophylla seeds.
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(a)
42.5 42.4 R² = 0.96
42.3
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41.5
41.1
40.9
41.0
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40.5
00 90 1801270 360 2450 540 3 4 5 6
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Irradiation power (W)
44 (b)
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43.5 43.2
43.1
43 42.6
42.5
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% Yield
41.4
41 40.8
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40.2
40
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0 2 4 6 8 10
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Fig. 3. Bio-oil yield of S. macrophylla seeds at variable (a) irradiation powers and (b)
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irradiation times.
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Fig. 4. Contour and 3D response surface plots showing the effects of irradiation time and
irradiation power to bio-oil yield.
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PT
RI
U SC
AN
M
Fig. 5. Diagnostic graph on the actual versus predicted bio-oil yield as influenced by
MWP.
D
TE
C EP
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(a)
Transmittance (%)
PT
RI
SC
Wavelength (cm-1)
U
(b)
AN
Transmittance (%)
M
D
TE
EP
Wavelength (cm-1)
Fig. 6. FTIR spectra of the extracted bio-oil from (a) microwave and (b) oven pretreated
C
seeds.
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