Waste Management 30 (2010) 799–803

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Waste Management
journal homepage: www.elsevier.com/locate/wasman

Biodiesel production from waste frying oils and its quality control
T. Sabudak a,*, M. Yildiz b
a
Department of Chemistry, Faculty of Science and Arts, Namik Kemal University, 59100 Tekirdag, Turkey
b
Biodiesel Energy Ind. Trd. Inc., Velimese Industry Region, Corlu, Tekirdag, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: The use of biodiesel as fuel from alternative sources has increased considerably over recent years, afford-
Accepted 7 January 2010 ing numerous environmental benefits. Biodiesel an alternative fuel for diesel engines is produced from
Available online 25 January 2010 renewable sources such as vegetable oils or animal fats. However, the high costs implicated in marketing
biodiesel constitute a major obstacle. To this regard therefore, the use of waste frying oils (WFO) should
produce a marked reduction in the cost of biodiesel due to the ready availability of WFO at a relatively
low price.
In the present study waste frying oils collected from several McDonald’s restaurants in Istanbul, were
used to produce biodiesel. Biodiesel from WFO was prepared by means of three different transesterifica-
tion processes: a one-step base-catalyzed, a two-step base-catalyzed and a two-step acid-catalyzed
transesterification followed by base transesterification. No detailed previous studies providing informa-
tion for a two-step acid-catalyzed transesterification followed by a base (CH3ONa) transesterification are
present in literature. Each reaction was allowed to take place with and without tetrahydrofuran added as
a co-solvent. Following production, three different procedures; washing with distilled water, dry wash
with magnesol and using ion-exchange resin were applied to purify biodiesel and the best outcome
determined. The biodiesel obtained to verify compliance with the European Standard 14214 (EN
14214), which also corresponds to Turkish Biodiesel Standards.
Ó 2010 Elsevier Ltd. All rights reserved.

1. Introduction use in biodiesel production, in view of their ready availability

The increasing production of waste frying oils (WFO) from
household and industrial sources is a growing problem worldwide.
Oils are generally poured down the drain, resulting in problems for
waste water treatment plants and energy loss, or integrated into
the food chain through animal feeding, thus becoming a potential
cause of human health problems (Costa Neto et al., 2000). Several
end-uses for this type of waste have been identified, including soap
manufacturing (Mittelbach and Tritthart, 1988) energy production
by means of anaerobic digestion, thermal cracking (Zaher, 2003),
and more recently the production of biodiesel, a fuel suited for
use as a petroleum diesel substitute for engines. However, the
majority of used oils are treated as waste materials frequently pro-
ducing both ecological and economical problems.
The catalytic conversion of waste frying oils by transesterifica-
tion into biodiesel results in marked economic and environmental
benefits. Biodiesel is biodegradable and nontoxic with low emis-
sion profiles thus being less, environmentally harmful than petro-
leum diesel. Biodiesel is capable of reducing the level of pollutants
as well as of potential carcinogens (Zhang et al., 2003; Demibas,
2002). Particularly, waste oils represent an economical option for
* Corresponding author. Tel.: +90 282 264 35 13; fax: +90 282 260 21 95.
E-mail address: tsabudak@yahoo.com (T. Sabudak).
and low cost (Kulkarni and Dalai, 2006).
Properties featured by used frying oils differ from those of
refined and crude oils. The presence of heat and water accelerates
the hydrolysis of tri-glycerides and increases the free fatty acid
(FFA) content (Fennema, 1985). FFA and water content elicit signif-
icant effects on the transesterification of glycerides with alcohols.
They also interfere with the separation of fatty acid esters and glyc-
erol. Thus, tri-glycerides containing high amounts of water and FFA
are not easily transesterified (Freedman et al., 1984). In literature,
several published studies have investigated biodiesel produced
from WFO by means of base or acid-catalyzed one-step transeste-
rification reactions and base-catalyzed two-step transesterification
reactions (Encinar et al., 2007; Caylı and Kusefoglu, 2008; Tomas-
evic and Siler-Marinkovic, 2003; Canakcı, 2007; Usta et al., 2005;
Felizardo et al., 2006; Ozbay et al., 2008). No previous studies pro-
viding detailed information on two-step acid-catalyzed transeste-
rification followed by base transesterification are available to date.
The aim of this study was to establish the most appropriate
method for use in the purification and characterization of biodiesel
from WFO. Waste frying oils, collected from several McDonald’s
restaurants by the Alternative Energy and Biodiesel Producers
Association (ALBIYOBIR) in Istanbul, were used in the production
of biodiesel using a one-step basic, two-step basic and two-step
acid-basic transesterification. Each transesterification reaction

0956-053X/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.wasman.2010.01.007
800 T. Sabudak, M. Yildiz / Waste Management 30 (2010) 799–803
took place with and without THF as a co-solvent. However, three
different purification procedures were applied in the production
of biodiesel. Seven parameters were assessed in the biodiesel pro-
duced to test for compliance with European Standard 14214.
2. Materials and methods
2.1. Materials
Waste frying oils were collected from several McDonald’s res-
taurants by ALBIYOBIR in Istanbul, Turkey. Two different waste fry-
ing oils with an FFA value 2% and 4.6%, respectively, were used in
the study. Both waste oils were used in all three processes, one-
step base, two-step base and two-step acid–base. Each process
was performed twice, with and without co-solvent. Methanol, tet-
rahydrofuran (THF) and sulphuric acid, were supplied by Merck
and magnesol (MgO:SiO2 (1:2.7)) from Dallas Group of America,
whilst sodium methoxide was obtained from Biodiesel Energy
Ind. Trd. Inc. Ion-exchange resins (PD-206) were purchased from
Purolite Chemical Company and filter (XZF-103) from Zeren Textile
Company.
2.2. Equipment
Transesterification was carried out in a 50 L conical reactor,
equipped with a 2500 watt resistance, a temperature controller,
a mechanical stirrer with two 56 rpm propellers, a circulation
pump (0.37 kw) for homogeneous mixing, a sampling valve and a
methanol-acid mixture valve.
In addition, density (EN ISO 3679), kinematic viscosity (EN ISO
3104), flash point (EN ISO 3679), water content (EN ISO 12937),
acid value (EN 14104), iodine value (EN 14111) and methyl ester
yield (EN 14103) tests were performed on biodiesel by using pyc-
nometry (KEM-DA-130N), viscometry (USL-ASTM viscometer),
flash point apparatus (Petrotest-Closed cup tester 30000-0), and
Karl-Fischer moisture titrator (KEM, MKC-50) and GC (Perkin El-
mer Clarus 500) with the conditions of inlet temperature:
240 °C, column flow: 2 mL/min, split flow: 50 mL/min, injection
volume: 1 lL, oven program initial temperature: 195 °C, hold
time (1): 0 min, hold time (2): 6 min, ramp (1): 5 °C/min, oven
program final temperature: 240 °C, column: Carbowax 20 M,
30 m  320 lm  0.25 lm film, carrier gas: Helium, FID tempera-
ture: 240 °C, H2 flow: 45 mL/min, air flow: 450 mL/min.
2.3. Transesterification procedure
The collected waste frying oil was first filtered to remove food
residues and then heated at 105–110 °C to remove water. WFO
contained 7% water and 1% solid particles. Water content was mea-
sured by Karl Fisher titration method and the percentage of solid
particular residue was obtained subsequent to weighing after fil-
tration percentage. Homogeneous WFO samples were used in the
production of biodiesel in a one-step basic, two-step basic and
two-step acid–base transesterification reaction. All transesterifica-
tion reactions were carried out both using THF as a co-solvent and
without THF. In the purification of biodiesel, three different meth-
ods, washing with distilled water, dry washing with magnesol and
treating with ion-exchange resin were applied. Seven parameters
were subsequently measured in biodiesel produced to test for
compliance with the European Standards for biodiesel EN 14214.
2.3.1. Ones step base-catalyzed transesterification
About 20 g (0.625 mol) of methanol and 1–1.5 g (0.0250–
0.0375 mol) of sodium hydroxide were used in the treatment of
virgin oil or waste frying oil featuring a free fatty acid content of
less than 1% per 100 g (0.12 mol) (Gerpen, 2005).
Free fatty acid content of the waste frying oil used in this study
was 4.6%. During the production process, 32 kg (37.6 mol) of waste
oils were mixed with 6.4 kg (200 mol) of methanol and 640 g
(11.85 mol) of sodium methoxide solution in methanol at a 30%
concentration. Waste frying oils were mixed with methanol and
sodium methoxide for 2 h at a temperature of 58 °C to allow the
transesterification reaction to take place (Acaroglu, 2003). How-
ever, at the end of the reaction time, neither biodiesel nor glycerine
was produced, due to the high free fatty acid content. The same
experiment was repeated using different waste frying oil samples
featuring, a 2% FFA content. Following completion of the reaction
the mixture was left to settle for approximately 10 h. Following
this period, the glycerine phase was drained out from the bottom
of the reactor. The biodiesel phase, separated from glycerine, was
heated to 110 °C and left for 30 min to permit evaporation of ex-
cess methanol. Magnesol was added to methanol-free biodiesel
and the mixture reactor stirred for 1 h in the reactor. The biodiesel
and magnesol mixture was then filtered.
2.3.2. Two-step base-catalyzed transesterification
In this method, the transesterification reaction took place in
two-steps. 75% of the methanol and methoxide was used at the
first step and the rest was used in the second step. Between the
first and the second steps, the mixture was left to settle for 2 h
and the glycerine phase subsequently separated out. In this study,
32 kg (37.6 mol) of WFO was used. For the reaction, 4.8 kg
(150 mol) of methanol and 480 g (8.88 mol) of sodium methoxide
were used at the first step and 1.6 kg (50 mol) of methanol and
160 g (2.96 mol) of sodium methoxide at the second step. Temper-
atures of both reaction media were adjusted to 58 °C, with each
reaction time lasting 1 h.
No biodiesel production was obtained from the experiment per-
formed using waste frying oil having an FFA value of 4.6%. Subse-
quently, the same procedure was applied using frying oil having
an FFA value of 2%. At the end of the reaction, the glycerine phase
was separated from biodiesel, and excess methanol was evapo-
rated. Methanol and glycerine free biodiesel was then mixed with
magnesol for 1 h and the mixture obtained subsequently filtered.
2.3.3. Two-step acid–base catalyzed transesterification
In this study, a two-step process was selected for biodiesel pro-
duction. The process was started with an acid-catalyzed esterifica-
tion procedure followed by base-catalyzed transesterification
process. Acid esterification, mainly used as a pretreatment process,
was performed as a first step remove FFA from waste frying oil.
During the esterification reaction, 32 kg (37.6 mol) of WFO, FFA va-
lue 4.6%, 3.3 kg (103.1 mol) methanol and 73 g (0.74 mol) of sul-
phuric acid (98%) were stirred for 1 h at a temperature of 58 °C.
During stirring, a 100 ml sample was taken every 15 min and
checked for FFA value. FFA values obtained for samples 3 and 4
were remarkably similar indicating that over a 1 h stirring period
the reactions reached an equilibrium. After 1 h, stirring was
stopped and the reaction mixture allowed to settle for 1 h. After
1 h settling, methanol, acid and water mixture phase was sepa-
rated from oil phase. The oil phase was analysed and new FFA va-
lue obtained as 2.2%. The same procedure was performed
repeatedly until an FFA value lower than 1% was achieved. For
the second reaction, 1.6 kg (50 mol) of methanol and 35 g
(0.35 mol) of sulphuric acid were used. Following this reaction
FFA value decreased to 0.7% and alcohol, water and acid mixture
phase was separated from the oil. Subsequent to phase separation,
6.4 kg (200 mol) of methanol and 640 g (11.85 mol) of 30% sodium
methoxide were added to oil and mixture was stirred for 1 h at
58 °C. On completion of the reaction, the mixture was left to settle
 T. Sabudak, M. Yildiz / Waste Management 30 (2010) 799–803 801

for 10 h. Glycerine phase was drained out from the bottom of the
reactor. The rest of the mixture, containing biodiesel and methanol,
was heated to evaporate excess methanol. After the evaporation,
magnesol was added to the methanol-free biodiesel and was mixed
for 1 h, subsequent to which the mixture was filtered to separate
biodiesel and magnesol.
2.3.4. Transesterification reactions with co-solvent (THF)
In the present study, tetrahydrofuran (THF) was used as a co-
solvent in each transesterification reaction. The amount of THF
used in each reaction was equal to the quantity of oil employed a
ratio of 1 kg THF to 1 kg waste frying oil (Boocock et al., 1998).
The results of the reactions are provided in Table 1.
2.3.5. Purification by washing with water
Washing was carried out using soft hot water at a temperature
of 50–60 °C. The amount of water used in the washing process was
equal to the quantity of biodiesel. Subsequent to washing biodiesel
was left to settle for 10 h and the water was then separated from
biodiesel. The washed biodiesel was dried by means of agitation
at 110 °C for 20 min.
2.3.6. Purification by magnesol
Magnesol corresponding to 1% the total amount of biodiesel
was added following separation from glycerine and methanol.
The resulting magnesol and biodiesel mixture was stirred for 1 h
at 70–80 °C. Magnesol was subsequently separated from biodiesel
by filtering.
2.3.7. Purification by ion-exchange resin
The flow velocity of biodiesel passing through the resin colon
was dependent on the amount of resin. In this process no temper-
ature limitations were applied when using biodiesel. The tempera-
ture of biodiesel passing through the ion-exchange resins should
however not exceed 150 °C. The present study was performed at
room temperature and biodiesel corresponding to one and half
times the amount of resin was passed through the ion-exchange
resins (Purolite-PD 206) at 1 h.
2.3.8. Characterization of the produced biodiesel
A series of tests were performed to characterize the properties
of the produced biodiesel according to EN 14214. These properties
include density (EN ISO 36799, viscosity (EN ISO 3104), flash point
(EN ISO 3679), water content (EN ISO 12937), acid number (EN
14104), iodine value (EN 14111) and methyl ester content (EN
14103).
According to the results shown in Table 1, the use of a co-sol-
vent does not produce a significant increase in reaction yield. The
highest yield increase obtained was 0.8%. From an economical
point of view, the use of THF in this study is not feasible as THF
is applied mainly to increase the solubility of methanol in oil. How-
ever, the mixing ability of the reactor is sufficient to achieve
homogenization of the methanol oil mixture.
3.2. Effect of purification methods on reaction yield
The biodiesel produced following transesterification reaction
may contain impurities such as soap, mono- di- tri-glycerides,
glycerine, methanol and salts. Washing with water, use of an
absorbent such as magnesol (this purification method is known
as dry wash) or ion-exchange resin can then be performed to
achieve separation impurities from biodiesel.
The effect of purification methods on transesterification reac-
tion yield is shown in Table 2. The lowest yield is obtained by
water wash and the highest yield by ion-exchange resin. The pres-
ent study revealed how use of ion-exchange resin proved to be the
best method in purification of biodiesel produced from waste fry-
ing oil.
3.3. Characterization of the produced biodiesel
In order to increase the commercial value of biodiesel, stan-
dards for fuel quality and control have been established by the
ASTM and European (EN) standards, among the most prominent
(Mahajan et al., 2007).
The biodiesel market is regulated by the Energy Market Regula-
tory Authority (EMRA) in Turkey. Marketed biodiesel must comply
with EN 14214 standards. Although 25 parameters are taken into
account by the Standard EN 14214, EMRA requires all biodiesel
producers to analyse a minimum of seven parameters; accordingly,
density, viscosity, flash point, water content, acid value, iodine va-
lue and methyl ester content were analysed in this study. The re-
sults of the analysis are illustrated in Tables 3–5. Limits reported
in these tables represent limit values of experimental methods
establish by EN 14214.
Table 1
The effect of reaction types without and with co-solvent on reaction yield.
Types of transesterification FFA values Yield (%)
reactions (%)
Without co- With co-
solvent solvent

3. Results and discussion One-step base 2 76.8 77.3

4.6 0 0

3.1. Effect of reaction types with and without co-solvent on reaction Two-step base 2 85 85.8
yield 4.6 0 0
Two-step acid–base 4.6 90.3 90.4
Vegetable oil does not dissolve in methanol; it is therefore nec-
essary to stir methanol and oil mixture well to obtain a homoge-
neous mixture. If the mixing process is not sufficient to
Table 2
homogenize the mixture, the reaction yield reaction decreases.
The effect of purification methods on reaction yield.
To solve mixing problems, a co-solvent such as n-hexane or tetra-
hydrofuran (THF) may be used (Boocock et al., 1998). Types of Yield before Yield after purification (%)
transesterification purification
The results obtained from transesterification reactions carried Washing Dry washing Ion-
reactions (%)
out with and without co-solvent, one-step basic, two-step basic with by magnesol exchange
water resin
and two-step acid–base transesterification, are shown in Table 1.
No biodiesel is produced by means of one-step and two-step One-step base 76.8 80.8 84.9 85.8
base transesterifation processes, from oil with FFA value 4.6%. Bio- Two-step base 85 91.0 92.3 93.4
Two-step acid– 90.3 95.6 96.9 98.4
diesel production yield, by two-step acid–base reaction process, is base
obtained as 90.4%.
802 T. Sabudak, M. Yildiz / Waste Management 30 (2010) 799–803

Table 3
The analysis results of produced biodiesel from a one-step base-catalyzed transesterification with co-solvent of WFO (FFA value: 2%).

Parameter Unit Limits Analysis results Experimental method

Minimum Maximum washing with water Dry washing by magnesol Ion-exchange resin
Density, 15 °C kg/m3 860 900 884 882 886 EN ISO 3679
Viscosity, 40 °C mm2/s 3.5 5 5.82 5.32 5.46 EN ISO 3104
Flash point °C 120 – 155 151 159 EN ISO 3679
Water content mg/kg – 500 422 637 381 EN ISO 12937
Fatty acid number mg KOH/g – 0.5 0.41 0.29 0.33 EN 14104
Iodine value g iodine/100 g – 120 106 106 106 EN 14111
Methyl ester % (m/m) 96.5 – 80.8 84.9 84.1 EN ISO 14103

Table 4
The analysis results of produced biodiesel from two-step base-catalyzed transesterification without co-solvent of WFO (FFA value: 2%).

Parameter Unit Limits Analysis Results Experimental method

Minimum Maximum Washing with water Dry washing by magnesol Ion-exchange resin
Density, 15 °C kg/m3 860 900 883 880 884 EN ISO 3679
Viscosity, 40 °C mm2/s 3.5 5 5.31 5.14 5.22 EN ISO 3104
Flash point °C 120 – 159 163 161 EN ISO 3679
Water content mg/kg – 500 398 526 317 EN ISO 12937
Fatty acid number mg KOH/g – 0.5 0.39 0.26 0.30 EN 14104
Iodine value g iodine / 100 g – 120 106 106 106 EN 14111
Methyl ester % (m/m) 96.5 – 91.0 92.3 91.7 EN ISO 14103

Table 5
The analysis results of produced biodiesel from two-step acid–base catalyzed transesterification without co-solvent of WFO (FFA value: 4.6%).

Parameter Unit Limits Analysis results Experimental method

Minimum Maximum Washing with water Dry washing by magnesol Ion-exchange resin
Density, 15 °C kg/m3 860 900 885 882 882 EN ISO 3679
Viscosity, 40 °C mm2/s 3.5 5 4.92 4.74 4.63 EN ISO 3104
Flash point °C 120 – 148 146 151 EN ISO 3679
Water content mg/kg – 500 422 487 372 EN ISO 12937
Fatty acid number mg KOH/g – 0.5 0.38 0.26 0.23 EN 14104
Iodine value g iodine/100 g – 120 106 106 106 EN 14111
Methyl ester % (m/m) 96.5 – 95.6 96.9 97.2 EN ISO 14103

4. Conclusions
Waste frying oil used in this study was obtained from several
McDonalds branches in Istanbul. Biodiesel was produced by three
different methods, one-step basic, two-step basic and two-step
acid-basic transesterification, each method being performed twice,
both with and without co-solvent (THF).
The effect of THF on reaction yield was found to be very low due
to the use of a reactor equipped with a mechanical agitator and cir-
culation pump for mixing, capable of homogenizing the mixture
sufficiently even without co-solvent. As an alternative to use of
co-solvent, which reduces reactor capacity and requires additional
energy for distillation of co-solvent, it is more economical to im-
prove the mixing ability of the reactor.
Three different purification methods, washing with water, addi-
tion of magnesol and ion-exchange resin were applied to biodiesel.
The most effective purification method was determined to be ion-
exchange resin. Although purification ability of magnesol was
comparable to that of ion-exchange resin, the clay used to filter
magnesol subsequently represents a toxic waste the disposal of
which is particularly costly.
Furthermore, purified biodiesel was analysed to check for com-
pliance with the standard EN 14214. The outcome of experiments
performed underlined the impossibility of producing, biodiesel
from waste frying oils with an FFA value higher than 2%, without
acid esterification. In the present study, biodiesel produced from
waste frying oil with an FFA value of 4.6% by means of two-step
acid base reactions and purification by ion-exchange resin met
requirements established by EN 14214. Consequently, the findings
obtained in the present study endorse the feasibility of producing
biodiesel by means of a two-step acid base process from WFO with
FFA value higher than 2% and ion-exchange resin for purification.
Acknowledgement
The authors would like to thank Biodiesel Energy Ind. Trd. Inc.
for the kind assistance provided during in this study.
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