Waste Management xxx (2014) xxxxxx

Contents lists available at ScienceDirect

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

Biodiesel production from vegetable oil and waste animal fats

in a pilot plant
Ertan Alptekin a,b, Mustafa Canakci a,b,, Huseyin Sanli b,c
a

Department of Automotive Engineering, Faculty of Technology, Kocaeli University, 41380 Izmit, Turkey
Alternative Fuels R&D Center, Kocaeli University, 41275 Izmit, Turkey
c
Golcuk Vocational High School, Kocaeli University, 41650 Golcuk, Turkey
b

a r t i c l e

i n f o

Article history:
Received 9 April 2014
Accepted 24 July 2014
Available online xxxx
Keywords:
Fleshing oil
Chicken fat
Corn oil
Pretreatment
Pilot plant
Biodiesel cost

a b s t r a c t
In this study, corn oil as vegetable oil, chicken fat and eshing oil as animal fats were used to produce
methyl ester in a biodiesel pilot plant. The FFA level of the corn oil was below 1% while those of animal
fats were too high to produce biodiesel via base catalyst. Therefore, it was needed to perform pretreatment reaction for the animal fats. For this aim, sulfuric acid was used as catalyst and methanol was used
as alcohol in the pretreatment reactions. After reducing the FFA level of the animal fats to less than 1%,
the transesterication reaction was completed with alkaline catalyst. Due to low FFA content of corn oil,
it was directly subjected to transesterication. Potassium hydroxide was used as catalyst and methanol
was used as alcohol for transesterication reactions. The fuel properties of methyl esters produced in the
biodiesel pilot plant were characterized and compared to EN 14214 and ASTM D6751 biodiesel standards.
According to the results, ester yield values of animal fat methyl esters were slightly lower than that of the
corn oil methyl ester (COME). The production cost of COME was higher than those of animal fat methyl
esters due to being high cost biodiesel feedstock. The fuel properties of produced methyl esters were
close to each other. Especially, the sulfur content and cold ow properties of the COME were lower than
those of animal fat methyl esters. The measured fuel properties of all produced methyl esters met ASTM
D6751 (S500) biodiesel fuel standards.
2014 Elsevier Ltd. All rights reserved.

1. Introduction
Biodiesel has received signicant attention in all countries since
it is nontoxic, biodegradable and renewable diesel fuel. Biodiesel is
generally produced from cooking vegetable oils. Using high-quality
virgin oils makes biodiesel more expensive than diesel fuel and it
causes to increase in vegetable oil prices. Therefore, low cost
feedstocks are needed and should be used in biodiesel production.
In Turkey, B2 (2% biodiesel, 98% diesel fuel) usage is excise tax free
for biodiesel produced from waste cooking vegetable oils.
However, there are different biodiesel feedstocks to be used in
the production. For example, rendered animal fats and leather
industry wastes are appealing feedstocks to produce biodiesel so
that there is no conict with food production.

Corresponding author at: Department of Automotive Engineering, Faculty of

Technology, Kocaeli University, 41380 Izmit, Turkey. Tel.: +90 262 3032202; fax:
+90 262 3032203.
E-mail
addresses:
mustafacanakci@hotmail.com,
canakci@kocaeli.edu.tr
(M. Canakci).

Chicken fat is a low cost feedstock for biodiesel production

compared to high-grade vegetable oils. It is extracted from chicken
wastes such as chicken feathers, blood, offal and trims after rendering process. Especially, chicken slaughterhouses not having a rendering plant have waste disposal problems. These wastes can be
evaluated in chicken fat producing. The chicken fat potential in
Turkey is considerably high. The number of chicken consumption
was about 1200 million in 2013 (TSI, 2014). If it is assumed that
25% of chicken amount are sent to rendering process and the fat
contents of rendering products are 1012%, there will be about
100 million kg of chicken fat per year. Leather industry wastes
are another feedstock for biodiesel production. Turkish leather
industry has taken a prominent place in the world leather trade
with its high export productivity. The number of animal skin production was about 10 million in 2013 (TSI, 2014). The leather
industry is one of the considerably polluting industries and it produces highly quantity of fat-originated solid and liquid wastes
while processing hides and skins (Ravindran and Sekaran, 2010).
Most of the solid waste in the leather production process is originated during the eshing procedure to remove esh and natural
fats from the hides and skins (Pecha et al., 2012). The fat content

http://dx.doi.org/10.1016/j.wasman.2014.07.019
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of leather industry wastes is remarkable. However, these wastes

are not evaluated effectively and there is almost no application
method to recover them. One way to recover the leather industry
wastes is using them as feedstock in the biodiesel production
due to their rich fat content (olak et al., 2005; Ozgunay et al.,
_ler et al., 2010).
2007a, b; Is
The pollution caused by the meat industry wastes increases
with the growing annual meat consumption. It may be reduced
and more valuable products can be obtained by converting them
to biodiesel. However, these waste oils and fats often contain signicant amounts of free fatty acid (FFA). FFAs may diminish the
biodiesel yield and complicate the biodiesel production because
they react with conventional alkaline catalysts such as potassium
and sodium hydroxide, and soaps are produced by this reaction.
Soaps prevent the separation of the ester, glycerin and wash water
(Canakci and Van Gerpen, 1999). Therefore, some additional
processes are required to get high biodiesel yield and standard
biodiesel fuel.
The FFA levels of the vegetable oils are generally lower than 1%
level while the FFA level of the rendering plant feedstock is generally between 5% and 25% (Canakci and Van Gerpen, 2001). The
researchers have suggested that the FFA level of the feedstock
should be reduced to less than 1% before using an alkaline catalyst
(Freedman et al., 1984; Liu, 1994). One way to recover the FFAs is
converting them to esters by using acid catalysts such as sulfuric
acid (Canakci and Van Gerpen, 2001) or strong base catalysts such
as tetramethylammonium hydroxide (Kolomaznik et al., 2009).
The acid catalysts are cheap and quite effective for converting FFAs
to esters. In biodiesel production, the acid-catalyzed process is
generally called as pretreatment. FFAs are converted to esters
through the pretreatment of the feedstock with high FFA and
thereby the FFA level reduces.
Many researches were performed on producing biodiesel from
waste vegetable oils and animal fats in laboratory scales
(Kolomaznik et al., 2009; Sabudak and Yildiz, 2010; Bhatti et al.,
2008). However, there are a partial number of studies on animal
fats especially with high FFAs in a pilot plant scale. Cunha et al.
studied (Cunha et al., 2009) the process of biodiesel production
in a pilot plant using beef tallow as biodiesel feedstock. The FFA
value of the beef tallow was about 0.75% on average. Therefore, it
was converted to biodiesel by transesterication reaction. They
used potassium hydroxide and methanol in the production. They
concluded that the alkaline transesterication of beef tallow produced high quality biodiesel with a good conversion rate. Canakci
and Van Gerpen (2003) evaluated two different animal fats with 9%
(yellow grease) and 40% (brown grease) FFA for biodiesel production in a pilot plant. After reducing the FFA level of the animal fats
by two step pretreatment with acid catalyst, they produced biodiesel by transesterication reactions via alkaline catalyst. The total
and free glycerin values of the animal fats biodiesels were suitable
to the biodiesel standards. Chitra et al. (2005) selected jatropha
curcus oil with 3.1% FFA for biodiesel production. After having
optimized concentration of methanol and NaOH in laboratory scale
experiments, the studies on large scale production of biodiesel
were performed in the biodiesel pilot plant. According to large
scale biodiesel production results, the average biodiesel yield was
obtained as 96%. The kinematic viscosity and specic gravity of
the jatropha biodiesel were found to be within the limit of
biodiesel standards.
In the previous studies (Alptekin and Canakci, 2010, 2011;
Alptekin et al., 2012), optimum reaction parameters were investigated to produce biodiesel from eshing oil and chicken fat. These
studies showed that FFA level of the high free fatty acid feedstock
could be decreased to below 1% in laboratory conditions. After
nding the optimum reaction parameters for small-scale transesterication of feedstocks, a pilot scale biodiesel production from

animal fats were aimed. The purpose of the present study is to produce biodiesel from vegetable oil and animal fats with high free fatty
acid in a biodiesel pilot plant. Therefore, the biodiesel production
processes in a pilot scale were investigated with corn oil, eshing
oil and chicken fat. The obtained methyl esters were characterized
by determining their fuel properties according to the standard test
methods, and fuel properties of the produced methyl esters were
compared to each other and biodiesel standards.
2. Materials and methods
In this study, corn oil, chicken fat and eshing oil were used as
feedstocks for biodiesel production. Corn oil was supplied from a
local market. The eshing oil was obtained from the solid wastes
recycle plant in Istanbul Leather Organized Industry in Istanbul,
TURKEY. It is known that there are two kinds of original eshing
which are green eshing and lime eshing (Sundar et al., 2011).
In this study, lime eshing oil was used. Chicken fat was acquired
from Beypili Chicken Slaughterhouse in Bolu, TURKEY. These animal fats are transformed into liquid form by a rendering process.
The corn oil and chicken fat were liquid at room temperature while
the eshing oil was in solid state at room temperature.
The initial target for the pretreatment is to reduce the FFA level
of feedstocks to less than 1%. Because the acid values of the animal
fats used in this study were greater than 2 mg KOH g 1, it was
needed to perform a pretreatment to the feedstocks. Due to low
acid value of corn oil, it was directly subjected to transesterication via base catalyst. Some measured properties of the oils are
shown in Table 1. The fatty acid compositions of the oils and
methyl esters are given in Table 2, which are important for the
determination of the mass balance in the process. According to
fatty acid compositions of the feedstocks, the total saturated fatty
acid compositions of corn oil, chicken fat and eshing oil are about
14%, 27% and 42%, respectively. On the other hand, saturated fatty
acid rates in the produced methyl esters remained almost the same
when compared with the respective feedstocks.
2.1. Pretreatment and transesterication process in the pilot plant
The optimum reaction parameters of small-scale transesterication of feedstocks were used in a pilot scale biodiesel production
from animal fats (Alptekin and Canakci, 2010, 2011; Alptekin et al.,
2012). In addition, corn oil was used in pilot scale biodiesel production to compare the fuel properties of vegetable oil and animal fats
methyl esters. The biodiesel pilot plant was assembled at the
Alternative Fuels Research and Development Center in Kocaeli
University. Biodiesels were produced in the pilot plant with the
capacity of about 100 kg per day. The schematic of the biodiesel
pilot plant is shown in Fig. 1. The feedstock tank (200 l) has electrical heaters to prevent solidication of feedstock especially for
eshing oil. All the feedstocks were ltered with 60-micron fuel
lter before transferring to feedstock tank.
Sulfuric acid and methanol were used for the pretreatment of
the eshing oil and chicken fat. Certain amounts of the feedstock
were transferred to main reaction (120 l) tank for pretreatment
reactions. The feedstock was dried under vacuum to remove any
potential water. The required amount of alcohol was transferred
from the alcohol tank (200 l) to methoxide tank (120 l). The acid
catalyst was added to the tank manually. Methanol and catalyst
were mixed in the tank named as methoxide tank. The reactant
amounts differ from each other due to different FFA levels of the
feedstocks and those will be mentioned in the next sections. The
alcohol and catalyst mixture were stirred about 20 min in the
methoxide tank and then it was transferred to the reaction tank
when the temperature of the feedstock in the reaction tank

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Table 1
Some properties of the chicken fat, eshing and corn oil.
Property

Unit

Density (at 15 C)
Kinematic viscosity (at 40 C)
Acid value
Heat of combustion
Sulfur content
Water content
Peroxide value
Iodine number
a

Chicken fat
3

kg m
mm2 s 1
mg KOH g 1
kJ kg 1
ppm
% mass
meq kg 1
g I.100 g 1

Fleshing oil

Corn oil

937.6
53.8
52.3
38,375
135
0.4
56.7
85

907.6
51.3
24.7
39,613
>990
0.3
4.2
52

922.5
32.8
0.3
39,651
6.3
0.1
6.1
115

Measured at 25 C.

Table 2
Fatty acid distributions of corn oil, eshing oil and chicken fat.
Product

Corn oil
Corn ME
Fleshing oil
Fleshing ME
Chicken fat
Chicken ME

Fatty acid distribution (%)

14:0

14:1

15:0

16:0

16:1

17:0

17:1

18:0

18:1

18:2

18:3

20:0

20:1

20:4

21:0

22:0

24:0

3.1
3.1
0.5
0.5

1.4
1.4

0.4
0.4

10.6
10.3
26.0
26.2
19.8
19.4

0.1

6.5
6.1
3.8
3.6

0.9
0.9
0.4
0.4

0.9
0.9

2.0
2.3
11.4
11.3
6.1
6.1

29.5
31.0
45.8
44.8
34.6
32.2

55.6
54.5
2.5
3.5
30.9
32.8

0.9
0.8
0.3
0.3
2.9
2.9

0.4
0.4

0.2
0.2
0.3
0.4

0.4
0.6

0.3
0.3

0.2
0.2

0.2
0.2

Fig. 1. Schematic view of the biodiesel pilot plant. 1. Feedstock tank, 2. Alcohol tank, 3. Methoxide tank, 4. Reaction tank, 5. Settling tank, 6. Washing tank, 7. Waste alcohol
tank, 8. Waste water tank, 9. Condenser, 10. Condense water inlet-outlet, 11. Sight glass, 12. To vacuum pump, 13. Washing water inlet.

reached to 60 C. The nal mixture was stirred for 1 h at 60 C. The

stirring speed was about 300 rpm and same for all reactions.
After the pretreatment reaction, the mixture was transferred to
settling tank to settle overnight, and then two phases was
occurred. The upper phase consists of the alcoholwateracid mixture and the other phase mainly consists of the esteried fatty
acids and initial triglyceride-animal fat (Canoira et al., 2008). The
upper phase was separated from the other phase. As known, when
the FFAs react with alcohol to form esters, water is also formed in
the products. Therefore, it is necessary to separate the water from
the pretreated material since it will inhibit further reaction.
Although methanolwateracid catalyst phase was removed by
settling, the esteroil mixture was subjected to a heating under
vacuum to remove any remaining water or methanol. To collect

the waste water and methanol, two stage drying process was performed manually. First, the esteroil mixture was subjected to a
heating at 6570 C to remove any remaining methanol for
2030 min (the valve of waste methanol tank was open). Then it
was heated to 105 C and kept at this temperature for 30 min to
remove any remaining water (the valve of waste water tank was
open). The recovered alcohol and water were controlled via the
sight glass as seen in Fig. 1. After drying process, the FFA level of
the feedstock was measured and recorded. Two steps pretreatment
reaction was performed for chicken fat because the FFA level could
not be decreased below 1% by the rst pretreatment.
After decreasing the FFA level of the feedstock below 1%, transesterication reaction was completed with alkaline catalysts for the
eshing oil and chicken fat. Because of the low FFA level of corn oil,

Please cite this article in press as: Alptekin, E., et al. Biodiesel production from vegetable oil and waste animal fats in a pilot plant. Waste Management
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it was directly used in transesterication reaction to produce biodiesel. For transesterication reactions, potassium hydroxide and
methanol were used. The transesterication processes were the
same as those of pretreatment experiments except for catalyst.
After the transesterication reaction, the reaction mixture transferred to the settle tank. The mixture was settled overnight and
the glycerin layer was separated. The ester layer was transferred
to the washing tank and it was washed with warm water. After
washing process, the methyl ester was sent to the main reaction
tank and it was subjected to a heating under vacuum to remove
excess alcohol and water as stated above, and then it was ltered
with 10-micron lter.
2.2. Characterization of fuel properties
The feedstocks and methyl esters were characterized in Alternative Fuels Research and Development Center in Kocaeli University
(AFRDC) and Marmara Research Center The Scientic and Technological Research Council of Turkey (MRC-TUBITAK). The test
methods used to determine the properties of the feedstocks and
methyl esters are given below (unless otherwise stated, the tests
were done in AFRDC);
Density (ASTM D4052), viscosity (ASTM D445), ash point
(ASTM D93), sulfur content (ASTM D2622), water content (EN
ISO 12937), iodine value (EN 14111), mono-, di- and triglyceride,
total-free glycerin (EN 14105 determined in MRC-TUBITAK),
methanol content (EN 14110), cold lter plug point (ASTM
D6371), acid value (AOCS Cd 3a-64), copper strip corrosion (ASTM
D130) and heat of combustion (ASTM D240), cetane number
(ASTM D613 determined in MRC-TUBITAK), fatty acid composition (IUPAC 2.301), peroxide value (AOCS Cd 8-53).
3. Results and discussion
In the process of producing biodiesel in the pilot plant, corn oil,
eshing oil and chicken fat were evaluated as feedstocks. Reaction
conditions were selected with taking into account of the properties
of feedstocks. Because the FFA levels of the animal fats were higher
than 1%, they were subjected to pretreatment reactions at the
beginning. After reducing the FFA level of the fats to below 1%,
transesterication reaction was completed with alkaline catalysts.
On the other hand, the corn oil methyl ester was produced by
transesterication due to having low content of FFA. Fuel properties of pretreated oils and methyl esters were characterized after
each reaction and detailed characterizations of the methyl esters
were done to check the suitability to the biodiesel standards. These
properties have been discussed in the Section 3.4.
3.1. Biodiesel production from corn oil
As seen in Table 1, the acid value of corn oil is below
2 mg KOH g 1 which is enough to use an alkaline catalyst for
transesterication reaction. The ingredient amounts used in the
transesterication for the corn oil were 7.7 kg methanol, 35 kg corn
oil (6:1 M ratio) and 0.35 kg KOH (1% of oil by weight). Reaction
time and temperature were 2 h and 60 C, respectively. The reaction parameters were selected by considering the previous studies
(Alptekin and Canakci, 2008a, 2009). Mean molecular weight of
corn oil was found to be about 875 g mol 1 calculated from the
fatty acid composition. The fatty acid composition for each oil
and methyl ester can be seen in Table 2. Ester yield is calculated
by dividing the ester amount to the corn oil amount used for
transesterication. After transesterication and purication
process, the ester yield was found to be 91% on mass. This value
is slightly lower than the value obtained in the laboratory

experiments. The reason for this may be higher amount of oil

and ester loss in the biodiesel pilot plant.

3.2. Biodiesel production from eshing oil

In the previous study (Alptekin et al., 2012), optimum reaction
parameters were investigated to produce biodiesel from eshing
oil in laboratory scale apparatus. Acid value of the eshing oil used
in the previous study was 24.3 mg KOH g 1 which corresponds to
FFA level of about 12.15%. FFA level of the feedstock was decreased
below 1% FFA level in the laboratory scale experiments by one step
pretreatment reaction. As seen in Table 1, the acid value of the
eshing oil used in this study was 24.7 mg KOH g 1. The pretreatment reaction parameters determined in the laboratory experiments were used in pilot scale biodiesel production because the
properties of the eshing oil used in the laboratory experiments
were very close to those of the eshing oil used in this study.
The pretreatment conditions for eshing oil were 30:1 alcohol
molar ratio and 10% sulfuric acid based on FFA level of the eshing
oil. In the calculations, the molecular weight of the FFA was calculated to be the average molecular weight of the fatty acids in the
eshing oil. The esterication process was repeated for two times
for the eshing oil. The ingredient amounts used in the pretreatment reactions for the eshing oil were given in Table 3a.
The acid value of the eshing oil was reduced from 24.7 to
1.9 mg KOH g 1 on average. This value is very close to the values
obtained in the laboratory experiments. In the pretreatment process, there was oil loss about ve percent of the eshing oil during
the alcohol-catalyst-water removing and drying process. In addition to acid value, some properties of the pretreated eshing oil
were characterized to understand the effects of pretreatment.
The pretreatment results were given in Table 3b. The density of
the eshing oil and pretreated eshing oil was measured at 25 C
because they were in solid form at room temperature. The viscosity, density and water content of the eshing oil reduced after the
pretreatment reaction. The fuel properties of the pretreated oils
were very close to each other. This situation shows the repeatability of the experiments. In this study, the sulfur content of eshing
oil was above 990 ppm which is the maximum measurement value
of the sulfur analyzer. The reason of high sulfur content of the
eshing oil is the results of the industrial process of the solid
wastes recycle plant where the eshing oil was obtained. This
means that sulfur content of the feedstock is important to get
low sulfur content biodiesel after transesterication.
After pretreatment reactions, the FFA level of the eshing oil
was 0.95% on average. The transesterication reaction parameters
were selected according to the previous study (Alptekin et al.,
2012). The ingredient amounts used in the transesterication reactions for the eshing oil were given in Table 3. The catalyst amount
was 1% weight of the initial amount of fat in the eshing oil.
Additionally, neutralization amount was used which was calculated from the reference (Van Gerpen et al., 2004). Molar ratio
between alcohol and fat-ester mixture was 7.5:1 based on the
initial fat amount in the eshing oil for the transesterication

Table 3a
Ingredient amounts used in the pretreatment and transesterication reactions of the
eshing oil.
Experiment 1

Pretreatment (kg)
Transesterication
(kg)
a

Experiment 2

Oil

Alcohol

Catalyst

Oil

Alcohol

Catalyst

50
45

21.1
11.3

0.62
0.4 + 0.1a

50
45

21.1
11.3

0.62
0.4 + 0.1a

Neutralization amount.

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Table 3b
Pretreatment results of the eshing oil.
Property

Unit
3

Density (25 C)
Viscosity (40 C)
Acid Value
Heat of Combustion
Sulfur Content
Water Content

kg m
mm2 s 1
mg KOH g
kJ kg 1
ppm
ppm

Fleshing Oil

Experiment 1

Experiment 2

907.6
51.3
24.7
39,613
>990
2650

901.1
22.98
1.906
39,415
>990
629

900.3
23.15
1.900
39,352
>990
770

reaction. Mean molecular weight of the eshing oil was found to be

about 850 g mol 1. After transesterication, the ester yield was
about 82% on average. Ester yield was calculated by dividing the
ester amount to the pretreated fat amount used for transesterication. Transesterication results were given in Table 3c. The fuel
properties of the eshing oil methyl ester were very close to each
other and t the international biodiesel standards.
3.3. Biodiesel production from chicken fat
Extensive studies to investigate the process for converting high
FFA chicken fat to biodiesel were described in the previous studies
(Alptekin and Canakci, 2010, 2011). The FFA level of the chicken fat
used in the previous studies was 12.45% which was decreased
below 1% in the laboratory scale experiments by one step pretreatment reaction. However, as seen in Table 1, the acid value of the
chicken fat used in this study was 52.3 mg KOH g 1 which corresponds to FFA level of about 26.15%. Therefore, for this study, several laboratory experiments were done to reduce the FFA level of
the chicken fat. In the previous study (Alptekin and Canakci,
2010), the optimum pretreatment reaction was found as 80 min
reaction time, 20% catalysts and 40:1 methanol molar ratio based
on the FFA level of the chicken fat to reduce the FFA level from
12.45% to below 1% by one step pretreatment reaction. These
reaction parameters were considered for the rst pretreatment
reaction. The reaction conditions were 1 h and 60 C for the rst
and second pretreatment reactions. The experiments were
performed in a laboratory scale apparatus. The process details for
laboratory experiments were given in the previous study
(Alptekin and Canakci, 2010).
The esterication process was repeated for amount of sulfuric
acid (20%) and different alcohol molar ratios (20:1, 30:1 and 40:1)
based on the FFA value of the chicken fat for 1 h at 60 C. According
to the results obtained experimentally, for 20% sulfuric acid and
methanol molar ratio of 20:1, 30:1 and 40:1, the FFA content was
reduced to 4.16%, 2.95% and 2.61%, respectively. Increasing the acid
catalysts amount in the pretreatment reaction causes more amount
of the loss of feedstock after the pretreatment. Lower feedstock
amount means lower biodiesel yield after transesterication. In
addition, there was almost no difference between methanol molar
ratio of 30:1 and 40:1 with 20% sulfuric acid catalyzed pretreatments. Therefore, instead of increasing acid catalyst or methanol
amount, the FFA level of the chicken fat was reduced below 1% by
two step pretreatment reactions. The pretreatment with 20%

Table 3c
Transesterication results of the eshing oil.
Property

Unit

Experiment 1

Experiment 2

Ester yield
Density (15 C)
Viscosity (40 C)
Acid value
Heat of combustion
Flash point

% mass
kg m 3
mm2 s 1
mg KOH g
kJ kg 1
C

81.6
876.7
4.69
0.27
39,917
168

82.3
876.6
4.71
0.30
39,849
168

sulfuric acid and methanol molar ratio of 30:1 for 1 h at 60 C

was thought to be sufcient for the rst pretreatment reaction to
get high ester yield after transesterication. Thus, these reaction
parameters were selected for the rst pretreatment.
For the second pretreatment reaction, the experiments were
performed with 10% sulfuric acid and 30:1 methanol molar ratio,
and the FFA level was decreased to 1.37%. It seemed that the FFA
level was not reached to less than 1%. Therefore, greater amount
of sulfuric acid and methanol molar ratio were used. The reaction
conditions of the next second pretreatment were the methanol
molar ratios of 40:1 and sulfuric acid amount of 15% for 1 h at
60 C. The FFA level was reduced to 0.81% after this reaction. This
value is enough to continue the process with transesterication
reaction. Therefore, these reaction parameters were selected for
the second pretreatment reaction.
The pretreatment reaction parameters determined in the laboratory experiments were used in the pilot scale biodiesel production.
The ingredient amounts used in the pretreatment reactions for the
chicken fat were given in Table 4a. After the rst pretreatment reaction in the biodiesel pilot plant, the acid value of the chicken fat was
reduced from 52.3 to 3.3 mg KOH g 1 on average. This value is close
to values obtained in the laboratory experiments but there is a little
difference between the acid value of the laboratory experiments and
pilot scale pretreatments. The reason of this situation was probably
effective and more homogenous mixing in the main reaction tank of
the biodiesel pilot plant for the rst pretreatment reaction. In the
pretreatment reactions, there were oil loss about 10% and 8% of
the chicken fat during the alcohol-catalyst-water removing and drying process for the rst and second pretreatment reactions, respectively. The pretreated chicken fat was subjected to the second
pretreatment reaction. The esterication process was repeated for
two times for the chicken fat. After the second pretreatment
reactions, the acid value of the chicken fat was reduced to
1.94 mg KOH g 1 on average.
The pretreatment results for chicken fat were given in Table 4b.
As seen in the table, the viscosity, density and water content of the
chicken fat were reduced by pretreatment reaction while the heat
of combustion of the chicken fat was slightly increased. According
to results, the fuel properties of the pretreated oils obtained after
two experiments were very close to each other. In this study, the
sulfur content of chicken fat was 135 ppm and the reason of high
sulfur content is probably the sulfur-containing compounds such
as protein (He et al., 2009). After the rst pretreatment reactions
in the biodiesel pilot plant, the sulfur content of chicken fat was
increased and measured approximately as 700 ppm on average.
This situation indicates that the alcoholwateracid catalyst
removing process after pretreatment is very important to get low
sulfur content pretreated chicken fat. However, the second pretreatment results showed that there was no signicant change in
the sulfur content values after the rst and second pretreatments.
Probably, some amount of sulfur cannot be separated with the
alcoholwateracid catalyst phase and still it is included in the
ester-initial triglyceride phase. As will be stated in the next section,
the sulfur content of the pretreated chicken fat was decreased to
lower values by transesterication reaction.

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Table 4a
Ingredient amounts used in the pretreatment and transesterication reactions of the chicken fat.
Experiment 1

1st Pretreatment (kg)

2nd Pretreatment (kg)
Transesterication (kg)
a

Experiment 2

Oil

Alcohol

Catalyst

Oil

Alcohol

Catalyst

45
40
35

40.5
3.1
6

2.4
0.1
0.27 + 0.08a

45
40
35

40.5
3.1
6

2.4
0.1
0.27 + 0.08a

Neutralization amount.

Table 4b
Pretreatment results of the chicken fat.
Experiment 1
Property

Unit
3

Density (15 C)
Viscosity (40 C)
Acid value
Heat of combustion
Sulfur content
Water content
a

kg m
mm2 s 1
mg KOH g
kJ kg 1
ppm
ppm

Experiment 2

Chicken fat

1st PT

2nd PTa

1st PTa

2nd PTa

937.6
53.81
52.30
38,375
135
4320

914.2
17.71
3.36
39,242
727
757

912.2
15.54
1.93
39,368
749
746

915.4
18.26
3.32
39,271
668
788

911.6
14.89
1.95
39,321
698
689

PT: pretreatment.

After two stage pretreatment reactions applied to chicken fat,

the FFA level was reduced to 0.97% on average. In the transesterication reactions, reaction parameters were chosen considering
the results in the previous study (Alptekin and Canakci, 2011).
The ingredient amounts used in the transesterication reactions
for the chicken fat were shown in Table 4a. The transesterication
were performed with the alkaline catalyst amount of 1% weight of
the initial triglyceride weight in the chicken fat at 6:1 M ratio
between methanol and fat-ester mixture. Mean molecular weight
of the chicken fat was calculated to be about 865 g mol 1. After
transesterication and purication process, the ester yield was
found to be about 81% on average. The transesterication results
were given in Table 4c. Fuel properties of the chicken fat methyl
esters were very close to each other.

3.4. Comparison of the fuel properties

After transesterication reactions, two different methyl esters
were obtained for eshing oil and chicken fat. Hence, these methyl
esters were mixed separately. Then, the fuel properties of all produced methyl esters were determined and compared to each other.
The fuel properties of the methyl esters produced in the pilot plant
and laboratory scale and related fuel specications in European
biodiesel standards (EN 14214) and American biodiesel standards
(ASTM D6751) were summarized in Table 5.
Density of a fuel is an important fuel characteristic and it
directly affects the engine performance. Many performance parameters such as cetane number and heating value are related with the
density (Tat and Van Gerpen, 2000; Ryan et al., 1984; Guru et al.,
2010). The densities of produced methyl esters were close to each
other and in the range of 876.7889.7 kg m 3 which were suitable

Table 4c
Transesterication results of the chicken fat.
Property

Unit

Experiment 1

Experiment 2

Ester yield
Density (15 C)
Viscosity (40 C)
Acid value
Heat of combustion
Flash point

% mass
kg m 3
mm2 s 1
mg KOH g
kJ kg 1
C

80.4
889.6
5.27
0.40
39,728
168

81.5
889.8
5.34
0.46
39,646
169

to biodiesel standards. Some of the physical properties limit the

use of biodiesel in diesel engines, especially viscosity (Encinar
et al., 2005). Viscosity inuences the quality of combustion
(Heywood, 1988; Lichty, 1967; Tate et al., 2006). In this study,
the viscosities of methyl esters varied in the range of 4.6
5.3 mm2 s 1. According to the results, the viscosity of chicken fat
methyl ester (CFME) was in accordance with ASTM D6751 biodiesel standard, while it was slightly higher than the viscosity limit of
the EN 14214 biodiesel standard. The researchers (Knothe and
Steidley, 2009) stated that the kinematic viscosity limit of EN
14214 biodiesel standard can affect the use of neat biodiesel from
waste oils as the kinematic viscosity of these fuels may exceed that
specied limit.
After transesterication, the ester may contain some unreacted
material such as triglyceride, residual alcohol, and residual catalyst. Beside, traces of glycerol which is separated from biodiesel
in the production process can also be found in the nal biodiesel
product. The total and free glycerin amounts of biodiesel are two
of the most important parameters to determine if the product is
ready for commercial applications. Since transesterication is a
stepwise process, monoglyceride and diglyceride formed as intermediates can also be found in biodiesel (Knothe, 2006; etinkaya
and Karaosmanoglu, 2004; Tyson, 2001). These parameters give
information about the purity of biodiesels. The glyceride values
of the produced methyl esters were very low and tted the biodiesel standards. The excess methanol used in the biodiesel production process must be removed. The allowable methanol content
level is specied in biodiesel standards as 0.2%. The methanol contents of the CFME, eshing oil methyl ester (FOME) and corn oil
methyl ester (COME) were 0.05%, 0.01% and 0.03%, respectively.
One of the most important advantages of biodiesel is its ash point
being higher than that of diesel fuel. The ash points of the produced methyl esters were measured to be around 169 C which
were much above the requirements and also higher than that of
diesel fuel (Alptekin and Canakci, 2008b).
The acid value is used to determine the amount of acid presents
in the fuel which has inuence on fuel aging. The EN 14214 and
ASTM D6751 have specied a maximum acid value of
0.5 mg KOH g 1 for biodiesel. The acid values of the COME, CFME
and FOME were 0.21, 0.28 and 0.43 mg KOH g 1, respectively.
The copper strip corrosion is used for the detection of the corrosiveness to copper of biodiesel fuels. The copper strip corrosion

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Table 5
Fuel properties of the produced methyl esters.
Property

Unit
3

Density (at 15 C)
Viscosity (at 40 C)
Flash point
Water content
Acid number
Monoglycerides
Diglycerides
Triglycerides
Free glycerin
Total glycerin

kg m
mm2 s 1
C
ppm
mg KOH g
% (mass)
% (mass)
% (mass)
% (mass)
% (mass)

Copper corrosion (3 h, at 50 C)
Heat of Combustion
Cetane Number
Methanol content
Sulfur content
Iodine value
CFPP

Degree of corrosion
kJ kg 1

% (mass)
mg kg 1
g I.100 g 1
C

EN 14214

ASTM D6751-12

FOME

FOME

860900
3.55.0
101 min
500 max
0.50 max
0.80 max
0.20 max
0.20 max
0.02 max
0.25 max

1.96.0
130 min

0.50 max
0.40 max

0.02 max
0.24 max

876.7
4.7
168
410
0.28
0.06
0.02
0.20
0.01
0.05

No 1 max

51 min
0.20 max
10 max
120 max

No 3 max

47 min
0.20 max
S1515 max S500500 max

No 1
39,892
58.8
0.01
138.1
53.6
10

CFME

CFME

875.5
4.77
175
326
0.32
0.27
0.09
0.04
0.01
0.10

889.7
5.3
169
440
0.43
0.02
0.05
0.06
0.008
0.03

No 1
39,954
NMa
0.01
141
61
11

No 1
39,693
52.3
0.05
81.5
95.5
3

COME

COME

883.0
4.94
172
NMa
0.22
0.56
0.09
0.12
0.02
0.19

886.0
4.6
169
440
0.21
0.06
0.17
0.06
0.01
0.06

884.0
4.18
192
NMa
0.17
NMa
NMa
NMa
0.013
0.17

No 1
40,173
NMa
0.01
NMa
NMa
2

No 1
39,878
54.2
0.03
4.1
119.3
5

NMa
NMa
NMa
NMa
NMa
NMa
1

NM: Not measured, 1: (Alptekin et al., 2012), 2: (Alptekin and Canakci, 2010, 2011), 3: (Alptekin and Canakci, 2008a, 2009).

result gathered with the produced methyl esters were the lowest
level of corrosiveness (No 1). Oxidation stability of biodiesel is
worse than petroleum diesel fuel. Therefore, biodiesel ages more
quickly than petroleum diesel fuel. The oxidation stability of produced methyl esters were not added to Table 5. Because, the oxidation stability of the methyl esters were determined according to
PetroOXYs Rapid Small Scale Oxidation Test (RSSOT) ASTM
D7545 method which has been approved but not incorporated into
ASTM fuel quality specications. However, the oxidation stability
of COME, CFME and FOME were about 0.11, 0.12 and 0.2 h respectively. On the other hand, the oxidation stability of diesel fuel was
about 1.52 h. The cetane number of a fuel shows the tendency of
that to self-ignite. Minimum cetane number of biodiesel is identied in ASTM D6751 as 47 while it is identied in EN 14214 as 51.
The cetane numbers of the produced methyl esters fullled both
biodiesel standards. The heat of combustion is a measure of the
energy available from the fuel. It is used for estimating the fuel
consumption compared to petroleum diesel fuel (Rashid et al.,
2009; Demirbas, 2000). The heat of combustion values of the produced methyl esters were around 40,000 kJ kg 1 which was
slightly lower than that of petroleum diesel fuel. Water in the fuel
builds up corrosion, and microbiological growth may occur at a
fuel-water interface. The ASTM D6751 and EN 14214 biodiesel
standards conrmed the highest water content value for biodiesel
of 500 ppm which were accomplished by the produced methyl
esters.
Iodine value is a measure of the degree of unsaturation of a vegetable oil or animal fat. The iodine value is not listed in ASTM
D6751 while it is listed in EN 14214 biodiesel standard to be maximum 120. The iodine value of the produced methyl esters tted
the biodiesel fuel standard value. The cold lter plugging point
(CFPP) is used to characterize the cold ow operability of a fuel
because it directly affects the utility of the fuel, especially in cold
climate conditions. The CFPP value of COME was much lower compared to CFME and FOME. The CFPP of FOME was +10 C which
were unacceptable to use these esters in the winter temperate
climates.
Sulfur content of a fuel has an effect on engine wear and deposits. Sulfur in the fuels is harmful for environmental and human
health, and it also affects emission values. Sulfur content must be
maximum 10 ppm for EN 14214 and it has two standard values
as S15 and S500 for ASTM D6751. S15 sulfur content standard
allows maximum to be 15 ppm, whereas S500 sulfur content standard allows maximum to be 500 ppm. Researchers (He et al., 2009)

Table 6a
The prices of the feedstocks, chemicals and utility costs.
Type of cost

Price ()

Corn oil (ton)

Chicken fat (ton)
Fleshing oil (ton)
Methanol (ton)
Sulfuric acid (ton)
Potassium hydroxide (ton)
Electrical (MW h)
Water (ton)

1182
338
338
2973
1689
6419
84
2.2

stated that when animal fats and waste vegetable oils are used for
biodiesel production, the sulfur content is expected to be higher
due to the presence of sulfur-containing compounds such as proteins. In this study, as seen in Table 1, the sulfur content of the
eshing oil and chicken fat were much higher compared to corn
oil. The reason of high sulfur content of the chicken fat may be
the sulfur containing protein which may be probably the keratin.
On the other hand, high sulfur content of the eshing oil results
from the industrial process of the solid wastes recycle plant where
the eshing oil was obtained because sulfuric acid is used in the
eshing oil production. After the rst pretreatment, the sulfur content of the chicken fat was increased. However, the sulfur content
of the pretreated chicken did not increase signicantly after the
second pretreatment reaction. The sulfur content of COME, FOME
and CFME were measured to be 138.1, 81.5 and 4.1 ppm, respectively. The sulfur content of the animal fat methyl esters tted
the ASTM D6751 (S500) biodiesel standard while they were not
suitable to EN 14214 biodiesel standard. The reason of the high sulfur content of these esters may be the sulfuric acid usage in the
biodiesel production. However, in some studies (olak et al.,
2005; Rashid et al., 2009), the sulfur content of the vegetable oil
or animal fat methyl esters did not t the EN 14214 sulfur standard
(10 ppm) although sulfuric acid was not used in those studies. This
shows that sulfur containing compounds may still be in the biodiesel after washing or purifying process. Therefore, water-washing or
other purifying methods are critical for sulfur removal.
The results showed that the fuel properties of the methyl esters
produced in the laboratory and pilot plant were a little different
but close to each other. The reason for this may be higher amount
of oil usage or production and rening process in the biodiesel pilot
plant. In addition, another reason may be that the fuel properties of

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Table 6b
The biodiesel production costs for each feedstock.
Type of methyl ester

Total cost (/l)

Methanol ()

Electricity ()

Water ()

Base catalyst ()

Acid catalyst ()

Feedstock ()

Chicken fat
Fleshing
Corn oil

1.40
1.13
1.62

5383
5511
3924

273
219
168

44
51
60

532
678
642

938
209

3380
3380
11,820

the used oils were not the entirely same for laboratory and pilot
scale experiments.
3.5. Economic analysis of biodiesel production
It is known that feedstock cost is the major problem to the market feasibility of biodiesel. In this study, low cost feedstocks such as
chicken fat and eshing oil were used for biodiesel production and
compared to vegetable oil based biodiesel. Therefore, the economic
analysis of biodiesel cost was conducted for a large scale biodiesel
plant (10 tons) to be more suitable to biodiesel industry. The operating costs of biodiesel plant were computed. The capital, plant
construction, and labor costs were not included. In the economic
analysis, glycerin recovery was not also included. However, the
excess methanol used in the pretreatment and transesterication
reactions was considered as economic gain. It was assumed that
90% of the methanol used in the pretreatment and 80% of the
excess methanol used in transesterication reactions were recovered. The prices of the feedstocks, chemicals and utility costs were
given in Table 6a. The prices of the chemicals and oils were
obtained from the local companies. The calculation was done based
on those prices. However, the prices may differ in any other country due to the currency difference. Therefore, it should be noted
that the nal costs of the biodiesels are valid only for Turkey.
The ingredient amounts for the pilot scale biodiesel production
were described in Tables 3a and 4a. Based on the amounts, electricity and water consumption in the pilot scale biodiesel production,
biodiesel costs were conducted for a large scale biodiesel plant (10
tons/day) which should be more suitable for biodiesel industry.
The obtained costs were shown in the Tables 6a and 6b.
Due to higher FFA content of chicken fat, it was necessary to use
higher amount of catalysts compared to eshing oil for pretreatment reactions as seen in Table 6b. Using higher amount of catalysts increases the price of CFME. This means that the FFA level
of the feedstock directly inuences the biodiesel cost. The operation cost of CFME is the lowest. However, it was still more expensive than the other methyl esters due to high cost feedstock. The
COME price was 15.7% and 43.1% higher when compared to CFME
and FOME, respectively.
4. Conclusion
The objective of this study was to produce biodiesel from
vegetable oil and low-cost animal fats with high free fatty acid in
a biodiesel pilot plant. For this aim, corn oil was used as vegetable
oil, while chicken fat and eshing oil were selected as animal fats.
These feedstocks were used for producing biodiesel in a pilot scale
and it was investigated that if any unique processes were required
to scale up from laboratory scale to pilot plant scale. According to
the results, there were no signicant differences in the fuel properties of methyl esters between laboratory and pilot plant experiments. Methyl esters produced in the laboratory and pilot plant
experiments showed similar properties. One or two step acid catalyzed pretreatment reaction process was effective in decreasing
the FFA level of the animal fats to less than 1%. After decreasing
the FFA level of the animal fats, alkaline catalyzed transesterication reactions resulted in good ester yields. Ester yield value of

the COME was slightly higher than those of animal fat methyl
esters. The fuel properties of produced methyl esters were close
to each other. The most apparent differences in the fuel properties
were the sulfur content and cold ow properties of the COME,
which were lower compared to animal fat methyl esters.
Especially, the cold property of the FOME was unacceptable to
use in winter climate. The cold ow properties of the FOME should
be improved with cold ow enhancers or it may be mixed with
petroleum diesel fuel which has better cold ow properties. Experimental results showed that the sulfur content of the biodiesel
feedstock is very important to get low sulfur content biodiesel after
transesterication. The sulfur content of COME was much lower
than those of animal fat methyl esters. On the other hand, the rst
sulfuric acid catalyzed pretreatment reaction increased the sulfur
content of pretreated fat. However, second pretreatment reaction
had almost no effect on the sulfur content of pretreated fat. Nevertheless, the animal fat methyl esters tted the ASTM D6751 (S500)
biodiesel fuel standards. According to the economic analysis, the
costs of biodiesels produced from corn oil, chicken fat and eshing
oil were 1.62 , 1.40 and 1.13 , respectively.
Acknowledgements
This study was supported by the grants from Scientic Research
Foundation of Kocaeli University and Izmit Municipality (Project
Nos. 2008/APP002 and 2011/37). The authors would like to thank
to Istanbul Leather Organized Industry and Beypili Chicken
Slaughterhouse (Bolu) managements for supplying the feedstocks.
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