Biofuels

ISSN: 1759-7269 (Print) 1759-7277 (Online) Journal homepage: http://www.tandfonline.com/loi/tbfu20

Energy analysis of extractive-transesterification of

algal lipids for biocrude production

Edith Martinez-Guerra & Veera Gnaneswar Gude

To cite this article: Edith Martinez-Guerra & Veera Gnaneswar Gude (2016): Energy analysis
of extractive-transesterification of algal lipids for biocrude production, Biofuels, DOI:
10.1080/17597269.2016.1195972

To link to this article: http://dx.doi.org/10.1080/17597269.2016.1195972

Published online: 28 Jun 2016.

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 BIOFUELS, 2016
http://dx.doi.org/10.1080/17597269.2016.1195972

Energy analysis of extractive-transesterification of algal lipids for biocrude

production
Edith Martinez-Guerra and Veera Gnaneswar Gude
Civil and Environmental Engineering Department, Mississippi State University, Mississippi State, MS 39762

ABSTRACT ARTICLE HISTORY

Algae biomass is the most promising feedstock for biofuel production since it can provide a Received 30 December 2015
sustainable route to achieve independence from fossil fuel sources. Energy-positive biofuel Accepted 4 March 2016
production from algal biomass has been the major goal for many researchers in recent years. KEYWORDS
The search for efficient extraction and chemical conversion methods that produce high energy Algae; biocrude, energy
ratios has become an important endeavor in this field. In this regard, microwaves and density; microwave; power
ultrasound have been utilized as convenient mechanisms in algal biodiesel production. intensity; ultrasonication
However, none of the studies reported on the energy analysis of the extraction and
transesterification methods. Energy analysis of the extractive-transesterification processes using
microwave (with ethanol and with ethanol and hexane as co-solvent) and ultrasound
Downloaded by [University of Regina] at 03:13 29 June 2016

irradiations to produce biocrude from microalgae (Chlorella sp.) is presented in this paper.
Power input and reaction volumes were varied to study the effects of power density and
intensity on the biocrude yields. Results from this analysis show that a biocrude yield higher
than 90% could be obtained with an energy input to output ratio of less than one when
microwave irradiation is used as the heating mechanism.

1. Introduction gallons of biodiesel (B100) were produced during the

first six months of 2015, which is higher than the data
The global energy demand is rising sharply with an
reported during the first six months of 2013 and 2014.
estimated additional energy consumption of 30% by
[6] Accordingly, the Renewable Fuel Standard (RFS)
the year 2040 as shown in Figure 1.[1,2] The dramatic
under the Environmental Protection Agency (EPA)
increase in fuel demand over the next 25 years can be
reported that the biodiesel produced during 2014 sup-
seen in Figure 1. This phenomenon is motivating the
ported approximately 60,000 jobs.[6] Therefore, by
research for renewable fuel production around the
2030, biofuels production is forecast to reach 6.5 Mb/d
world. This opportunity has also become a challenge
in comparison to its production in 2010 (1.8 Mb/d) indi-
for many researchers in diverse disciplines. The expec-
cating that the need and supply are forecasted to
tation of a new energy source has led these research-
increase tremendously in a near future.[1,7]
ers to explore not only for the ideal feedstock and the
Among various biodiesel feedstocks, algal biomass
most efficient process, but also for the policies to
can produce much higher quantities of oils than terres-
enhance the production of renewable energy sources.
trial oil plants [8] and algae biomass can be directly
Among various biofuels, biodiesel from biomass seems
converted into energy.[9,10] Algal biodiesel production
to be the most attractive option since it could poten-
has attracted common interest within the scientific
tially reduce the adverse environmental impacts of fos-
and industrial fields. However, algal biodiesel produc-
sil fuels while meeting the rising demands for
tion has to overcome many hurdles to become com-
transportation fuels. The major technical advantages of
mercially feasible. Despite the well-known and well-
biodiesel from biomass over petrodiesel include inher-
established advantages of algal biomass for biodiesel
ent lubricity, low toxicity, derivation from a renewable
production, the entire biodiesel production process
and domestic feedstock, superior flash point and bio-
must be improved to attain higher energy benefits.
degradability, negligible sulfur content, and lower
There are several steps to convert microalgae to bio-
exhaust emissions.[3] Biodiesel has a few disadvan-
diesel, which include biomass screening, cultivation,
tages relative to petrodiesel such as higher feedstock
harvesting, drying, lipid extraction, and oil to biodiesel
cost and limited availability, inferior oxidative stability,
conversion. Every step in algal biodiesel production is
and inferior cold flow properties.[3 5]
energy intensive, for example, the drying step takes up
According to the data reported from the United
to 89% of the energy input required and 70 75% of
States National Biodiesel Board (NBB), 594 million

CONTACT Edith Martinez-Guerra Gude@cee.msstate.edu; Veera Gnaneswar Gude Gudevg@gmail.com

© 2016 Informa UK Limited, trading as Taylor & Francis Group

 2 E. MARTINEZ-GUERRA AND V. G. GUDE
Figure 1. Present and predicted world liquid fuels consump-
Downloaded by [University of Regina] at 03:13 29 June 2016
tion until year 2040.
total processing cost.[11,12] According to Lardon et al.,
[13] the total energy consumed for dry algal biomass
conversion to biodiesel is 106.4 MJ/kg and produced
biodiesel with an energy content of 103.8 MJ/kg with a
net energy balance of ¡2.6 MJ/kg. On the other hand,
algal biodiesel production from dry biomass consumed
a total energy of 41.4 MJ/kg and produced biodiesel
with an energy content of 146.8 MJ/kg with a positive
net energy balance of 105 MJ/kg.[13] In order to
reduce the energy burden of dewatering and drying, it
is proposed to process residual biomass further for bio-
energy (such as bioethanol or biogas via fermentative
processes) or valuable biochemical product formation.
[14] Moreover, lipid extraction and conversion steps
are also major obstacles for the commercialization of
microalgal biodiesel because of the high cost and
energy input required.[15,16] The economics of algal
biodiesel production mainly depends upon the energy
utilized for the processing of biomass and the type of
lipid extraction process used.[17,18] Extractive transes-
terification or in-situ transesterification is recom-
mended as the most efficient process to produce
biodiesel [19,20] in a single reactor using algal cells,
and without having to follow the traditional, indepen-
dent separate process of extraction and conversion.
This process significantly reduces the energy consump-
tion; however in situ transesterification has the disad-
vantages of excess solvent and catalyst requirements.
[21] For this reason, use of a co-solvent such as hexane
could enhance the extraction process while reducing
the alcohol requirement. Also, the biomass conversion
to biocrude production requires excessive reactant/sol-
vent to move the reaction forward due to the presence
of other biological cell materials. If the co-solvent can
be recovered and reused in a closed loop
configuration, the solvent intensity of the process
could be diminished to a great extent.
In this study, extractive-transesterification of algal
lipids directly from dry algal biomass was conducted
using microwave irradiation with and without hexane
and ultrasound individually. An ideal biofuel production
process should provide for higher energy benefits
while reducing the environmental footprint. Energy
investment into the production scheme should be
reduced to increase the net energy benefit. Many stud-
ies reported the microwave and ultrasound non-con-
ventional techniques as promising methods to extract
algal oils and reported energy consumption for the
extraction process. However, few articles reported the
total energy output from the extractive-transesterifica-
tion process, emphasizing mainly on the cultivation
energy input and output. The goal of this research is to
elucidate the relationship between the energy density
and power intensity of the two non-conventional
methods in extractive-transesterification of algal lipids.
This article discusses the relationships between the
biocrude yield and the energy ratios for producing
algal biocrude at different process conditions. Optimum
conditions for achieving energy positive biodiesel
production have been identified which are crucial for
large scale process development. Algal biocrude was
produced using microwave (with and without hexane
as a solvent) and direct ultrasound irradiations, applied
individually. Specific energy consumption during the
extraction-conversion process with reference to avail-
able energy in the algal biocrude was discussed. The
following sections describe the experimental proce-
dures, process optimization and comparative studies
and the energy analysis of the single-step, extractive-
transesterification process.
2. Extractive-transesterification process
2.1. Materials
Dry algae biomass (Chlorella sp.) was purchased from a
commercial producer. The algal biomass has the fol-
lowing composition: 99% pure Chlorella biomass with
protein 52%, carbohydrates 16%, and others including
lipids, vitamins, and chlorophyll A. Ethanol (>99%
purity), hexane (98% C extra pure), and sodium
hydroxide (99.5% purity) were purchased from Cole
Palmer. All reagents and standards used in the GC-MS
and GC-FID analysis were purchased from Fisher
Scientific.
2.2. Lipid extractive-transesterification
During the extractive-transesterification process, a
microwave (MW) (manufactured by Columbia Interna-
tional TechnologiesÒ ) reactor with temperature and
power control functions was used. The MW reactor

was equipped with a reflux condenser to provide for
condensation of evaporating solvent mixture. To
enhance mass transfer, a magnetic stirrer was used to
ensure uniform mixing with a constant mixing speed
for all the experiments. The three-neck custom-fabri-
cated reaction vessels used during the MW experi-
ments were also provided by Columbia International
Technologies as well as the NO-MS100 ultrasonicator.
Each sample was repeated three times to verify data
accuracy. The MW and ultrasound (US) were cooled
with a fan after each experiment. The power output of
MW and US was 700 and 1000 W, respectively. The
ultrasonic frequency was 25 kHz and the horn is made
of titanium alloy.
Four grams of dry algae powder was added to the
premixed homogeneous solution of ethanol (and hex-
ane) and sodium hydroxide catalyst. The mixture was
then exposed to MW or US irradiation under a matrix
of conditions including: 3 7 minutes reaction time;
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dry algae to ethanol (wt./vol.) ratios of 1:6 1:15 (24,
36, 48, and 60 mL) and ethanol to hexane ratios of
24:8, 24:16, 24:24, and 24:30 mL; power output rates of
10 100% (based on MW 700 W). Similar experiments
were conducted with reaction mixture containing
24 mL of ethanol and 24 mL of hexane to study the
effect of hexane as a solvent. Hexane use as a solvent
was done using only microwave irradiations. The sam-
ples were left to settle and cooled using a fan and
immediately placed in a freezer before the analysis GC-
FID (MS) analysis.
2.3. Biodiesel analysis and fatty acid ethyl esters
(FAEE, biodiesel) composition
FAEE analysis was carried out on a Varian Gas Chroma-
tography (GC) with cool on column injection and FID
detection as required by ASTM 6584 method for B100
to measure the FAEE conversion. The FAEE composi-
tions in ethanol and hexane phases (before separation)
were analyzed using an Agilent 6890 gas chromato-
graph equipped with a flame ionization detector (Agi-
lent, Santa Clara, CA, USA). The column used was a
100 m x 0.25 mm x 0.2 mm Supelco SP 2380 capillary
column (Supelco, Bellefonte, PA, USA) with stabilized
poly (90% biscyanopropyl/10% cyanopropylphenyl)
siloxane as the stationary phase.
3. Results and discussion
3.1. MW-US extractive-transesterification process
optimization
Under the process optimization studies, two different
single-step extractive-transesterification methods using
MW irradiation were evaluated: (1) with ethanol as a sol-
vent and a reactant and sodium hydroxide as catalyst;
and (2) with ethanol as a reactant and hexane as a
BIOFUELS 3
solvent (sodium hydroxide as catalyst). Ethanol is essen-
tial for transesterification of lipids extracted in the pro-
cess into biodiesel. Hexane was used as solvent for two
purposes: (1) to enhance extraction of lipids by dissolv-
ing them in hexane; and (2) to control thermal effects
of microwaves under continuous power output because
hexane is a non-polar solvent with negligible dielectric
constant unaffected by the microwave field. Biodiesel
yields from these two methods were compared. The
maximum lipid yield was similar for MW with and with-
out hexane, 20.1%, while the FAEE conversion of the
algal lipids were 96.2 and 94.3%, respectively. The algae
biomass to ethanol molar ratio of 1:250 500 and
2.0 2.5% catalyst with reaction times around six
minutes were determined as optimum conditions for
MW and MW hexane methods. A comparative study of
microwave and ultrasound effects on the algal biodiesel
production via extractive-transesterification was also
conducted. For the microwave and ultrasound irradia-
tions, the following were determined as optimum: (1)
microwaves 1:12 algae to ethanol (wt./vol.) or 1:500
(molar) ratio; 2 wt.% catalyst; 5 6 min reaction time at
350 W microwave power; and (2) ultrasound 1:6 9
algae to ethanol (wt./vol.) or 1:250 375 (molar) ratio;
2 wt.% catalyst; six minutes reaction time at 490 W
ultrasound power. The highest FAEE yields for micro-
wave and ultrasound methods were 96.2 and 95.0%,
respectively. In comparison, the ultrasound method
resulted in higher FAEE yield and conversion at low sol-
vent ratios while microwaves were able to produce bet-
ter results at lower power levels compared to
ultrasound.
3.2. Effect of energy density on biocrude yields
In this process, energy density can be defined as the
amount of energy supplied per unit volume of the
sample. The energy density can be controlled either by
varying the power levels or by the sample volume. The
energy density from MW and US irradiations were cal-
culated when power output or sample volume was var-
ied in these reactions. The power output was varied
between 70 and 700 W at different percentages (i.e.
10 100% based on the maximum output of 700 W) of
MW power output. The energy densities from different
power output are shown in Figure 2, for MW using eth-
anol as a solvent and reactant (Figure 2a), for MW using
ethanol as a reactant and hexane as a solvent (Figure
2b), and for ultrasound reactions (Figure 2c). Figure 2d
depicts the biocrude yields in relation to specific
energy density for all conditions. It can be noticed that
higher energy density does not necessarily improve
the biocrude yield. On the contrary, the biocrude yield
decreased with increase in the energy density. As
shown, the optimal energy density for both MW (with
and without hexane) and US is approximately 2 kJ/mL.
Additionally, it should be noted that the energy
 4 E. MARTINEZ-GUERRA AND V. G. GUDE
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Figure 2. Effect of power output (between 70 W and 700 W) expressed as energy density (kJ/mL) with sample volume fixed at
48 mL on biocrude yields: (a) for MW alone; (b) for MW-Hex; (c) for US irradiation alone; and (d) comparative yield.
densities for US reactions take into account the entire
reaction time (5 min), however the actual energy densi-
ties for US reactions are approximately 16% lower since
pulse sonication was used. The pulse time used was 5 s
ON and 1 s OFF, which means that during five minutes
reaction time, the US irradiation was not supplied for
50 seconds. Therefore, it reduces the total energy
consumption.
Similar to Figure 2, the energy densities for different
reactant-solvent (ethanol-hexane) ratios are shown in
Figure 3 (the quantities are described under Section
2.2). Figures 3a, b and c show the biocrude yield pro-
files for MW, MW-Hex, and US separately at different
energy densities and Figure 3d shows the combined
results. It was noticed that US requires higher energy
density (3.75 kJ/mL) to achieve the highest biocrude
yield of 94.5%, while MW needs approximately 2 kJ/mL
to obtain 96.1% biocrude using only ethanol and about
91% using ethanol and hexane (MW-Hex). Even
though, as mentioned earlier, pulse sonication reduces
energy consumption because of its pulse settings, it
still consumed twice as much energy required by MW
to produce similar results. It is worth mentioning that
although MW and MW-Hexane follow the same trend,
the energy density for MW-Hexane is much lower than
using ethanol. Therefore, the addition of hexane as sol-
vent reduces the use of ethanol which cannot be
recovered easily after the transesterification step. Hex-
ane can be recycled, but it also reduces the energy
density to produce a reasonable biocrude yield. The
optimum energy density ranges between 2 3 kJ/mL
for all the microwave and ultrasound extractive-trans-
esterification reactions in both power controlled and
volume controlled reactions.
3.3. Ultrasonication: power (ultrasonic) intensity
and power density effects
Power density, similar to energy intensity, is the power
applied per unit volume. Power or ultrasonic intensity
is the amount of ultrasound effect applied on a given
surface area of the reactor.[22 24] As noticed in Figure
4, the power density and ultrasonic intensity follow a
similar trend; however, the ultrasound intensities are
less than the power applied per volume. The ultrasonic
intensity was calculated by measuring the diameter of
the reactor used for the extractive-transesterification
process, and then the different power percentages
were divided by the area. Since ultrasound requires
more power input compared microwaves, the biocrude

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Figure 3. Effect of sample volume (between 24 mL and 60 mL) expressed as energy density kJ/mL (power fixed at 350 W) on bio-
crude yields: (a) for MW alone; (b) for MW-Hex; (c) for US irradiation alone; and (d) comparative yield.
yields were lower at low ultrasound power density or
intensity. However, as highlighted on the plot, higher
power density or power intensity are neither favorable
to enhance the biocrude yields (less than 90%). The
highest biocrude yield of 95% was obtained at a power
intensity of 24.2 W/cm2 and a power density of
9.4 W/mL. An optimum range can be noticed on the
encircled area (right circle) where several process
points lie within, the power density ranges from
4 12 W/mL (10 24 W/cm2 power intensity) where the
biocrude yields are higher than 90% which is a reason-
able yield.
Figure 4. Power density and power intensity effects on algal
biocrude yields using ultrasound irradiation.
BIOFUELS 5
3.4. Specific energy consumption
The energy ratio is often used to determine the effi-
ciency of a specific technology. Moreover, energy ratio
is a common method of quantifying biodiesel’s renew-
ability.[25] It is expressed as the ratio of energy input
to energy output. The lower the ratio, the higher the
energy benefits from the process. The energy ratios for
MW and US reactions were calculated, and are shown
in Figure 5 (for MW) and Figure 6 (for US). These figures
show the energy ratio as well as the energy consumed
during the extractive-transesterification process. High
energy liquid biofuels usually have energy content
higher than 30 MJ/kg. During GC-MS analysis, the pres-
ence of aromatic hydrocarbons, long-chain fatty acids,
nitrogen heterocycles, and alcohols in the biocrude
were observed, which agrees with the observations
made by Pandey et al.[26] Pandey et al. reported that
the biocrude contains a carbon content of typically
70 75%, an oxygen content of 10 16%, a nitrogen
content of 4 6%, and the energy value typically
ranges from 33.4 to 39.9 MJ/kg [26]. Therefore, the con-
sumed energy was divided by an average energy con-
tent of 36 MJ/kg of algal biocrude obtained from the
authors’ experience and literature review. Ideally, the
desired energy ratio must be the lowest possible,
smaller than one. The shaded region (see Figure 5 and
 6 E. MARTINEZ-GUERRA AND V. G. GUDE
Figure 5. Energy ratio and consumed energy using MW (with and without hexane) irradiation.
Figure 6) shows that one data point for both micro-
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wave and ultrasound irradiations fall within the ideal
ratio, less than one. A biocrude yield of 91.3% for MW
was obtained for an energy ratio of 0.97 MJ/MJ, and it
is a higher yield than the 90.8% yield at a ratio of
9.98 MJ/MJ. The highest biodiesel yield (90.8%) using
MW-Hex was obtained at an energy ratio of
4.35 MJ/MJ. Unexpectedly, the energy ratio using MW-
Hex was not lower than 1 MJ/MJ for any of the condi-
tions. The lowest energy ratio for MW-Hex was
1.16 MJ/MJ with a biocrude yield of 86.5%. A similar
study (with different catalyst, Li4SiO4) was presented
by Dai et al. [27] where MW irradiations with a power
output of 1000 W were applied to a sample of 5 g of
microalgal biomass and an oil/methanol ratio of 1:18
for 4 h; however, in this case the energy ratio exceeded
20 MJ/MJ with a conversion of 76.2%.
Even though ultrasound can enhance the molecular
energy of solvents in the sample as well as strong pen-
etration to destroy the cell wall so that the solvent can
Figure 6. Energy ratio and consumed energy using ultrasound irradiation.
efficiently extract the lipids,[27 29] the results were
not as anticipated. The biocrude yield (67.7%) for an
energy ratio of less than one (0.85 MJ/MJ) was not
favorable when using direct sonication because of the
heating limitation by the ultrasound. The results only
include the reaction time when the ultrasound waves
were applied, which means the pulse off time was not
included in the calculations. Dai et al. [27] also com-
pared MW and US irradiations. Similar to this work,
they concluded that MW irradiations yielded higher
conversion percentages with microalgae biomass. Sim-
ilarly, Teo and Idris [30] compared MW with a water
bath heating method and determined that higher
energy ratios were obtained using MW. However, the
previously mentioned experiments results were much
lower than the results presented in this work because
direct sonication was used instead of water bath heat-
ing and indirect sonication. It must be acknowledged
that these calculations were performed for the produc-
tion of biocrude, which is less than the total energy

embedded in pure biodiesel. Therefore, further investi-
gation is still required to produce pure biodiesel from
algal biomass at an acceptable energy ratio. Another
assumption made in this study is that the algal biomass
is dried using freely available solar energy and has not
been considered in the energy analysis. Similar analysis
can be performed for wet algae extraction which might
prove to be a more energy efficient process. Micro-
waves and ultrasound together can provide a synergis-
tic effect that can help enhance biocrude yields and
increase energy returns.[31]
4. Conclusions
Microwaves and ultrasound irradiation enhance the
biocrude yields in extractive-transesterification in short
reaction times. Both techniques are effective for extrac-
tive-transesterification of microalgae, but have some
limitations that need further investigation (and experi-
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mental work) before planning on a commercial scale
production to minimize energy consumption. The
energy balance of microalgae biodiesel production
depends on the process technique and it is species-
specific. Eliminating energy-intensive algal drying pro-
cess could be an alternative to reduce the overall cost
of algal biodiesel production. Energy ratios for extrac-
tive-transesterification methods should be further
studied at a larger scale to determine the real benefits
of microwaves and ultrasound irradiations.
Acknowledgments
This research was supported in part by the United States
Environmental Protection Agency (USEPA). This research was
also supported by the Office of Research and Economic
Development (ORED), the Bagley College of Engineering
(BCoE), and the Department of Civil and Environmental Engi-
neering (CEE) at Mississippi State University. The authors
would like to thank Mrs. Marta Amirsadeghi and Dr. Todd
French of the Swalm School of Chemical Engineering for their
help with GC-MS analysis.
Disclosure statement
No potential conflict of interest was reported by the authors.
Funding
US Environmental Protection Agency [grant number
SU835519].
ORCID
Edith Martinez-Guerra http://orcid.org/0000-0002-7689-
3736
BIOFUELS 7
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