b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 2 8 6 7 e2 8 7 3

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http://www.elsevier.com/locate/biombioe

Refined soybean oil transesterification enhanced by

sonication
G. Riva, G. Toscano, E. Foppa Pedretti, D. Duca*
Dipartimento di Scienze Alimentari, AgroIngegneristiche, Fisiche, Economico Agrarie e del Territorio, Universita` Politecnica delle Marche,
Via Brecce Bianche, 60131 Ancona (AN), Italy

article info

abstract

Article history:

Biofuels are of great topical interest, especially in the light of recent European directives.

Received 6 October 2009

Biodiesel is both already available and thoroughly regulated. A critical aspect of the trans-

Received in revised form

esterification process, used in biodiesel production, is maximization of the contact surface

7 March 2011

between reagents. This is currently achieved using discontinuous processes with mechanical

Accepted 10 March 2011

agitation, which however afford poor mixing efficiency. Ultrasound appears to be an effective

Available online 7 April 2011

method to enhance mixing intensity. The aim of this work was to assess the advantages
offered by this technique, especially in terms of process velocity. For this purpose a small

Keywords:

scale experimental apparatus for biodiesel production integrated with a modular ultrasound

FAME

system was set up. Plant dimension and energy inputs were chosen to enable eventual

Glycine max

industrial implementation. Plant performances were assessed as the velocity of oil conver-

Ultrasound

sion to fatty acids methyl esters. The product was analyzed according to EN 14105. In general,

Transesterification

the efficiency of ultrasound in increasing reaction velocity was markedly affected by residual
triglyceride content. Conversion rates in line with EN 14214 and ASTM D6751 standard
specifications, which allow a maximum residual triglycerides content of 0.20%, were obtained
with reductions in reaction time of about 20%. In less stringent conversion conditions, e.g. 3%
triglycerides, the reaction time was roughly halved. Below 1% of triglycerides residues sonication should be interrupted and the process continued with conventional agitation.
2011 Elsevier Ltd. All rights reserved.

1.

Introduction

Vegetable oil transesterification is based on the reaction of

triglycerides (TG) with an alcohol, usually methanol, in the
presence of an acid or base, resulting in production of fatty
acid esters and glycerol. Stoichiometrically, the reaction
requires a 3:1 alcohol to TG molar ratio. However, since
transesterification is an equilibrium process, a surplus of
alcohol is always employed to drive the reaction to completion
and achieve ester production [1].
Several studies have been conducted to find ways to cut
production cost, for instance by using exhaust oil, different

catalysts, fixed bed reactors and continuous processes [2e7].

The most widely studied catalysts are NaOH and KOH, which
are commonly used in industrial production of biodiesel.
The transesterification reaction is characterized by a first
slow stage, a second fast stage, and a slowing down until
achievement of final equilibrium [8]. The alcoholysis process
is affected by several factors, mainly catalyst type and its
concentration, alcohol type, alcohol:oil molar ratio, reaction
temperature, amount of free fatty acids, water content and
mixing intensity [9,10]. Since TG and alcohols are not
completely miscible, the reaction takes place mainly at the
phase interface through a very slow process. Mass transfer of

* Corresponding author. Tel.: 39 71 2204297; fax: 39 71 2204167.

E-mail addresses: g.riva@univpm.it (G. Riva), g.toscano@univpm.it (G. Toscano), e.foppa@univpm.it (E. Foppa Pedretti),
d.duca@univpm.it (D. Duca).
0961-9534/$ e see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biombioe.2011.03.023

2868

b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 2 8 6 7 e2 8 7 3

Fig. 1 e Schematic representation of the experimental biodiesel plant.

TG from the oil phase to the oil-methanol interface therefore

critically affects reaction velocity. Consequently, mixing
intensity is highly important. The process currently adopted
in several industrial plants is based on mixing and heating.
Low-frequency ultrasound (US) is widely used in industry to
obtain emulsions from immiscible fluids. The chemical effects
of US stem from non-linear acoustic phenomena, especially

cavitation. When sound passes through a fluid, expansion

(negative pressure) and compression waves (positive pressure)
are generated, with formation and collapse of bubbles saturated with vapors of solvent, solute and previously dissolved
gases. At high US intensities inertial cavitation promotes the
rapid growth of small cavities; some of these grow to a size that
makes them unstable and eventually collapse violently, with

Fig. 2 e Schematic representation of the two types of sonication cells employed.

b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 2 8 6 7 e2 8 7 3

Table 1 e Operative parameters of cell A tests.

Test
A0
A1
A2
A3
A4
A5
A6

Sonication
Off
On
On
On
On
On
On (reduced cell)

Area (cm2) Power (W) Pressure (kPa)

e
12.5
12.5
9.0
9.0
3.8
3.8

e
240
420
320
560
320
510

101
101
202
101
202
101
202

obliteration of phase boundaries and formation of an emulsion

through the action of ultrasonic jets that impinge one liquid to
another, resulting in increased mass transport rates [11]. This
property is known as liquid jet effect. Cavitation therefore
effectively concentrates the US energy to a chemically usable
form. Another effect of US is mixing by acoustic streaming,
where a macroscopic flow is induced in the fluid via absorption
of sound waves by the reaction medium [12].
Mixing efficiency is improved by sonication [13]. The study
of continuous vegetable oil transesterification with US has
suggested that the technique could successfully replace
conventional mixing-heating, enabling 3- to 5-fold greater
reaction velocities in the initial stage compared with
mechanical agitation. Unfortunately, none of the several
works on the subject enable direct transfer of the results to
industrial production.
In the final step of the reaction, methanolysis is increasingly
slow until equilibrium, despite a greater interface area. The loss
of velocity is determined by falling methanol concentrations
and rising concentrations of glycerin and esters [14]. There are
no data on the effect of US on the final step of the reaction.
We studied different settings of the main operative
parameters on reaction conditions using a US-based transesterification system designed to be applied on an industrial
scale. Special emphasis was placed on integrating US with
traditional mechanical agitation. The effect of US on the final
stage of the reaction, on which existing data are scarce, was
also investigated.

2.

Material and methods

2.1.

Description of the experimental reactor

(University of Marche, Ancona, Italy) to study process variables,

assess the process velocity that could be achieved, and evaluate
the scope for their utilization in a full scale industrial plant.
The system consists of:
-

two reactors, each with a theoretical maximum capacity of 10 l;

a heater, to heat the reactor;
a variable capacity gear pump for reagent recirculation;
valves to regulate product pressure and recirculation;
sampling systems;
an evaporative condensation system for alcohol recovery;
a sonication cell;
a UIP1000hd US apparatus (Hielscher Ultrasonics GmbH,
Teltow, Germany);
- a device to measure the power absorbed by the US system.
The plant can perform a complete batch cycle in a preset
time or work in continuous flow using both reactors.

2.2.

Experimental plan

To make the tests comparable, all trials were run with identical amounts of reagents: 4000 g commercial refined soybean
oil (water content < 500 mg kg1 and free fatty acids
< 1 mg KOH g1); 869 g anhydrous methanol (Panreac),
providing a 6:1 alcohol:oil ratio, and 24 g sodium methoxide
(Sigma-Aldrich), or 0.6 % of the weight of oil as the catalyst.
The reaction temperature was kept constant (60  C). Samples
for conversion rate analyses were taken (tc) 20, 40, 60, 120, and
180 min from the introduction of the alcohol-catalyst mixture
in the reactor. All tests were run in triplicate.
The following operative parameters were changed in the
experiments:
- configuration of the recirculation and of the coupling to the
US system;
- sonotrode front size (12.5, 9.0, 3.8, and 2.2 cm2);

An experimental Fatty Acids Methyl Esters (FAME) production

plant (Fig. 1) combining US and conventional agitation was
constructed at the Biomass Lab, of SAIFET Department

Table 2 e Operative parameters of cell B tests.

Test Sonication Area Power Pressure Sonication Process
(kPa)
(min)
duration
(cm2) (W)
(min)
B0
B1
B2
B3

Off
On
On
On

e
2.2
2.2
2.2

e
110
110
110

101
101
101
101

0
180
20
40

180
180
180
180

2869

Fig. 3 e Sonication of vegetable oil.

2870

b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 2 8 6 7 e2 8 7 3

Fig. 4 e Residual TG content in cell B tests (the dashed line indicates the maximum level allowed by EN 14214 standard).

- power absorbed by the US system (from 110 to 560 W);

- circuit pressure (101 kPa and 202 kPa);
- capacity of the recirculation pump (0.8 and 4.0 dm3 min1).
The tests were performed to assess and optimize the
performance of the US system without changing mixing
conditions, which are related to the conventional recirculation system. Two different sonication cells, A and B (Fig. 2),
were used to run 7 and 4 transesterification tests, respectively
(Tables 1and 2).
The tests with the cell A have been performed for planning
purposes and to overcome the lack of literature on the
implementation of ultrasound systems in the transesterification processes and on the factors that drive the
process. Therefore, this preliminary investigation aimed to
highlight the main factors to be studied further.
Cell A was obtained with a standard Tee joint, where the
sonotrode was mounted. In one of the tests the internal
volume was reduced by inserting a steel pipe to direct the flow
toward the active surface of the sonotrode (test A6).
All tests were performed at maximum pump capacity
(4.0 dm3 min1), changing only the main operative parameters
affecting the sonication process: power absorbed by the US
generator; pressure of the sonication cell, and sonotrode front
area.
Analysis of the tests performed with cell A and of the
images of some sonication tests (Fig. 3), including some run by

other authors [15], prompted a number of modifications aimed

at improving fluid-wave interactions, which led to the design
and construction of cell B. Given the results of the preliminary
investigation it was decided to study with the cell B only the
effect of US application.
Cell B featured a steel pipe, with the sonotrode on one end
and a bore pipe (smaller than the one fitted in cell A) directing
the optimized flow of reagents toward the active surface of the
sonotrode (i.e. its frontal area), on the other. Tests were conducted using the parameters listed in Table 2. The sonotrode
was 16.8 mm in diameter and 2.2 cm2 in front. A steel pipe
6 mm in diameter was fitted to replace a part of the circuit to
compensate for the lower velocity in the tubing of the circuit
and the consequently lower turbulence. This enabled the fluid
to be poured into the zone of the sonication cell that was
closest to the cavitation.
To make the results useful for full plant scale, data on the
energy absorption and the main operative parameters of
traditional industrial plants were collected, better to understand the impact of US on overall energy consumption in the
transesterification step.
The recirculation pump capacity:volume of pumped fluid
ratio (0.8 dm3 min1) and the number of changes/hour of the
small scale plant were then comparable to those of real
reference plants. Optimization of the energy parameters was
achieved using the lowest power setting of the US generator
that was detectable by our measurement system (110 W).

Table 3 e Cell A test data.

tc (min)

20
40
60
120
180

A0(%)

A1(%)

A2(%)

A3(%)

A4(%)

A5(%)

A6(%)

MG

DG

TG

MG

DG

TG

MG

DG

TG

MG

DG

TG

MG

DG

TG

MG

DG

TG

MG

DG

TG

2.19
1.50
0.93
0.69
0.71

3.31
1.69
0.87
0.34
0.20

5.60
2.48
1.51
0.44
0.19

1.55
1.08
0.86
0.67
0.71

1.82
1.12
0.73
0.34
0.18

2.77
1.84
0.98
0.26
0.15

1.03
0.81
0.89
0.55
0.50

1.34
0.79
0.96
0.27
0.18

2.07
1.13
0.84
0.26
0.11

1.26
0.83
0.64
0.70
0.51

1.53
0.82
0.48
0.24
0.12

2.63
1.36
0.72
0.15
0.10

1.05
0.76
0.70
0.52
0.54

1.53
0.75
0.52
0.24
0.19

2.04
1.06
0.69
0.18
0.07

1.39
0.97
0.84
0.74
0.70

1.49
0.90
0.56
0.32
0.23

2.54
1.56
0.77
0.21
0.12

0.86
0.68
0.58
0.48
0.40

1.14
0.73
0.43
0.27
0.21

2.08
1.17
0.51
0.20
0.10

2871

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Table 4 e Cell B test data.

tc
(min)
20
40
60
120
180

2.3.

B0(%)

B1(%)

B2(%)

B3(%)

MG

DG

TG

MG

DG

TG

MG

DG

TG

MG

DG

TG

1.85
0.72
0.62
0.45
0.42

2.86
0.91
0.51
0.22
0.17

4.58
1.51
0.69
0.20
0.09

1.05
0.65
0.56
0.42
0.39

1.59
0.67
0.35
0.17
0.08

2.73
0.97
0.47
0.13
0.04

1.32
0.91
0.69
0.56
0.44

1.70
0.99
0.73
0.25
0.16

2.79
1.48
0.85
0.20
0.10

1.04
0.67
0.61
0.44
0.42

1.59
0.70
0.40
0.18
0.09

2.75
0.99
0.54
0.15
0.06

Sample treatment and analysis

3.

After collection each sample was added with acetic acid to

neutralize the catalyst and block the reaction; esters and
glycerin were immediately separated by centrifugation. The
ester sample was prepared for gas chromatography analysis
of monoglyceride (MG), diglyceride (DG) and TG residues
according to the EN 14105 method. Glycerol and glycerides
were transformed into more volatile silylated derivatives in
presence of pyridine and N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA). The silylated derivatives were
analyzed by gas chromatography, using a machine fitted with
a short capillary column with thin film thickness, an oncolumn injector, and a flame ionization detector. After calibration, quantification was carried out in the presence of the
standard 1,2,3-tricaproylglycerol.

Results

Test results, i.e. residual MG, DG and TG, are reported separately for cell A and cell B (means of three experiments).
However, of the data related to the velocity of conversion of oil
to FAME only residual TG content, which is sufficiently
informative, is reported for the sake of clarity and due to space
constraints for cell B (Fig. 4).

3.1.

Cell A test results

For cell B, the trial was set up in a randomised complete block

design. One-way analysis of variance (ANOVA) was performed
using SAS. When significant F-tests were obtained, means
separation was achieved using a Least Significant Difference
(LSD) test at the 0.05-probability level.

MG, DG and TG content in the tests performed in cell A are

shown in relation to reaction time (Table 3).
A general reduction in reaction time was noted already
when comparing the tests employing US and those with
conventional agitation.
Analysis of residual TG would seem to indicate better
conversion in the tests under pressure (A2, A4, and A6) already
at 20 min (ca. 2.00% vs 2.60%) compared with those without
pressure (A1, A3, and A5). These preliminary results are in line
with previous reports [11] describing faster and more violent
bubble collapse in this condition, where greater contact
between reagents enhances the first phase of the reaction.

Table 5 e Comparison of conventional and

conventional D US transesterification to produce a FAME
meeting the EN 14214 and ASTM D6751 standards.

Table 6 e Comparison of conventional and

conventional D 40 min US transesterification to produce
a FAME meeting the EN 14214 and ASTM D6751
standards.

Difference
Ultrasound
(%)

Conventional

Difference
process
Ultrasound
(%)

2.4.

Statistical analysis

Conventional
process
Compliance with EN
14214 and
ASTM D6751
Temperature ( C)
Reaction time (min)
Residual TG (%)
EE consumption for
US (kWh l1)
EE consumption for
transesterification
(kWh l1)
Other EE
consumptions
(kWh l1)
Total EE
consumption
(kWh l1)

Yes

Yes

60
120
0.20
e

60
95
0.20
0.0396

e
21
e
e

0.0100

0.0079

0.0302

0.0302

0.0402

0.0777

93

Compliance with EN
14214
and ASTM D6751
Temperature ( C)
Reaction time (min)
Residual TG (%)
EE consumption for
US (kWh l1)
EE consumption for
transesterification
(kWh l1)
Other EE
consumptions
(kWh l1)
Total EE
consumption
(kWh l1)

Yes

Yes

60
120
0.20
e

60
95 (40 US)
0.20
0.0167

e
21
e
e

0.0100

0.0079

0.0302

0.0302

0.0402

0.0548

36

2872

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Table 7 e Comparison of conventional and

conventional D US transesterification to produce a FAME
with 3.00% residual TG content.
Conventional

Difference
process
Ultrasound
(%)
Compliance with EN
14214 and ASTM
D6751
Temperature ( C)
Reaction time (min)
Residual TG (%)
EE consumption for
US (kWh l1)
EE consumption for t
ransesterification
(kWh l1)
Other EE
consumptions
(kWh l1)
Total EE
consumption
(kWh l1)

No

No

60
30
3.00
e

60
18
3.00
0.0075

e
40
e
e

0.0025

0.0015

0.0302

0.0302

0.0327

0.0392

20

of cell A accelerated the process irrespective of sonication (as

shown by comparison of tests B0 and A0).
The rates of conversion laid down by the EN 14214 standard
were reached in ca. 120 min in the test without US (B0) and in
95e100 min in the one where US was used throughout (B1).
The maximum time gain with these settings is thus 20% of the
total.
The test where US were applied only in the first 20 min,
followed by conventional agitation (B2), yielded interesting
results. Observation of the trend of residual TG content (Fig. 4)
showed an unexpected and marked slowing of reaction
velocity for 20 min after the interruption of sonication, with
implications for overall process velocity. This has been
confirmed by statistical analysis which showed no significant
differences after 40 min of reaction between B0 and B2 tests.
In contrast, the test where US was applied over the first
40 min followed by agitation (B3) exhibited a trend statistically
similar to the one where US was applied throughout (B1),
demonstrating that beyond such duration US neither accelerates nor slows down the reaction.

3.3.
From 60 min such differences then tended to zero. In addition,
the tests under pressure (202 kPa) were associated with 40%
more power use by the same US generator.
An interesting indication is that the system used in test A6
achieved the best conversion rate at 60 min, highlighting the
value of directing the reagent flow to the area closest to the
cavitation, as noted in previous reports [15]. However, the TG
content envisaged by the EN 14214 standard (0.20%) was
consistently reached in ca. 120 min also in test A6.

3.2.

Cell B test results

Cell B test data (Table 4) show that replacement of the first

portion of the circuit with a 6 mm pipe and use of cell B instead

Table 8 e Comparison of conventional and

conventional D US transesterification to produce a FAME
with 4.00% residual TG content.
Conventional

Difference
process
Ultrasound
(%)
Complying with
EN 14214 and
ASTM D6751
Temperature ( C)
Reaction time (min)
Residual TG (%)
EE consumption for
US (kWh l1)
EE consumption for
transesterification
(kWh l1)
Other EE
consumptions
(kWh l1)
Total EE
consumption
(kWh l1)

No

No

60
24
4.00
e

60
11
4.00
0.0046

e
54
e
e

0.0020

0.0009

0.0302

0.0302

0.0322

0.0357

11

Considerations

The experimental data, the electrical consumption of real

plants and the transesterification literature were analyzed.
The biodiesel producers report an electrical energy (EE)
consumption for the transesterification step ranging from 9 to
40 kWh t1 of biodiesel (equivalent to 0.00774e0.0344 kWh l1).
This range is mostly related to plant dimension and is
however in line with the 30 kWh t1 used in the well-towheels analysis of the JEC for the European context [16]. The
unit value of 0.01 kWh l1 adopted in our case, which is also
within that range, was calculated by taking into account the
consumption of a real plant with a 20 m3 reactor and a 400 kW
US system, which is proportional to the 110 W employed in the
tests with our experimental reactor.
The data predicted for different conversion levels are listed
in Tables 5e8. Each item relates to EE consumption per liter of
FAME produced; other consumptions are independent of the
conversion step and calculated by taking into account the
consumption of the same real plant.
Production of a FAME meeting the EN 14214 and ASTM
D6751 standards applying US throughout uses twice the EE as
the conventional process and saves about 20% in reaction
time. EE consumption can be significantly reduced by applying
US only over the first 40 min (Table 6), corresponding to the
step where US was seen to be most efficient in our tests. In this
case total EE consumption increases by a mere 36%. A shorter
duration of the sonication would be deleterious, given the
outcome of the test B2.
Production of FAME with higher residual TG levels than
those required by the two standards (Tables 7 and 8) is more
interesting, as US involves a more efficient energy use and has
a smaller impact on total EE consumption per liter of product.
At the same time the differences in reaction time between the
conventional process and the one using US are larger, virtually
doubling production capacity. In particular, production aiming at a residual TG content of 4.00% (Table 8) involves
a decrease in reaction time from 24 to 11 min, with a difference of 54%.

b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 2 8 6 7 e2 8 7 3

4.

Conclusions

In the EU automotive biodiesel is regulated by EN 14214, which

lays down specific conversion limits. These, therefore, define
when a transesterification reaction is to be considered as
completed.
Since one objective of the present work was to transfer the
method to an industrial plant, tests were run to obtain the
maximum possible time gain using sustainable energy inputs.
Thus, the tests run in cell B used the lowest power setting of the
US generator (110 W). Data analysis indicated that sonication
reduced the reaction time by about 20%. This was due both to the
power setting and to use of the 6 mm pipes, which enhanced
process efficiency irrespective of US application by accelerating
the first phase of the reaction, where sonication acts most efficiently. In conclusion, the more efficient the transesterification
process by conventional agitation, the smaller the velocity gains
that can be achieved by sonication. Integration of US into the
process is valuable in systems characterized by low reaction
velocity. The present results also indicate that sonication should
be halted at a residual TG content of 1.00%.
Linear transfer of these data to a 20 m3 cycle1 batch plant
would require an approximately 400 kW US generator to
achieve the same reaction time gains. Sonication for the first
40 min of the reaction would involve 36% greater electricity
consumption compared with the conventional process,
delivering a 20% gain in reaction time.

Acknowledgments
The authors are grateful to C&T S.p.A. for the financial support
and to SIBE S.r.l. (Spin-Off of Universita` Politecnica delle
Marche) for sample analysis.

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