Waste Management 34 (2014) 2146–2154

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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
b
Alternative Fuels R&D Center, Kocaeli University, 41275 Izmit, Turkey
c
Golcuk Vocational High School, Kocaeli University, 41650 Golcuk, Turkey

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

Article history: In this study, corn oil as vegetable oil, chicken fat and fleshing oil as animal fats were used to produce
Received 9 April 2014 methyl ester in a biodiesel pilot plant. The FFA level of the corn oil was below 1% while those of animal
Accepted 24 July 2014 fats were too high to produce biodiesel via base catalyst. Therefore, it was needed to perform pretreat-
Available online 21 August 2014
ment 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%,
Keywords: the transesterification reaction was completed with alkaline catalyst. Due to low FFA content of corn oil,
Fleshing oil
it was directly subjected to transesterification. Potassium hydroxide was used as catalyst and methanol
Chicken fat
Corn oil
was used as alcohol for transesterification reactions. The fuel properties of methyl esters produced in the
Pretreatment biodiesel pilot plant were characterized and compared to EN 14214 and ASTM D6751 biodiesel standards.
Pilot plant According to the results, ester yield values of animal fat methyl esters were slightly lower than that of the
Biodiesel cost 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 flow 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.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction Chicken fat is a low cost feedstock for biodiesel production

Biodiesel has received significant 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 conflict 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).
compared to high-grade vegetable oils. It is extracted from chicken
wastes such as chicken feathers, blood, offal and trims after render-
ing process. Especially, chicken slaughterhouses not having a ren-
dering 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 10–12%, 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 pro-
duction was about 10 million in 2013 (TSI, 2014). The leather
industry is one of the considerably polluting industries and it pro-
duces 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 origi-
nated during the fleshing procedure to remove flesh 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
0956-053X/Ó 2014 Elsevier Ltd. All rights reserved.
 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154
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 (Çolak et al., 2005; Ozgunay et al.,
_ßler 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 sig-
nificant 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 gener-
ally 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 transesterification reaction. They
used potassium hydroxide and methanol in the production. They
concluded that the alkaline transesterification of beef tallow pro-
duced 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 produc-
tion in a pilot plant. After reducing the FFA level of the animal fats
by two step pretreatment with acid catalyst, they produced biodie-
sel by transesterification 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 specific 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 investi-
gated to produce biodiesel from fleshing 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
finding the optimum reaction parameters for small-scale transeste-
rification of feedstocks, a pilot scale biodiesel production from
2147
animal fats were aimed. The purpose of the present study is to pro-
duce 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, fleshing
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 fleshing oil were used as
feedstocks for biodiesel production. Corn oil was supplied from a
local market. The fleshing 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 fleshing
which are green fleshing and lime fleshing (Sundar et al., 2011).
In this study, lime fleshing oil was used. Chicken fat was acquired
from Beypiliç Chicken Slaughterhouse in Bolu, TURKEY. These ani-
mal fats are transformed into liquid form by a rendering process.
The corn oil and chicken fat were liquid at room temperature while
the fleshing 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 transesterifica-
tion 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 fleshing 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 transesterification process in the pilot plant
The optimum reaction parameters of small-scale transesterifi-
cation 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 produc-
tion 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 electri-
cal heaters to prevent solidification of feedstock especially for
fleshing oil. All the feedstocks were filtered with 60-micron fuel
filter before transferring to feedstock tank.
Sulfuric acid and methanol were used for the pretreatment of
the fleshing 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
2148 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154

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

Property Unit Chicken fat Fleshing oil Corn oil

3 a
Density (at 15 °C) kg m 937.6 907.6 922.5
Kinematic viscosity (at 40 °C) mm2 s 1 53.8 51.3 32.8
Acid value mg KOH g 1 52.3 24.7 0.3
Heat of combustion kJ kg 1 38,375 39,613 39,651
Sulfur content ppm 135 >990 6.3
Water content % mass 0.4 0.3 0.1
Peroxide value meq kg 1 56.7 4.2 6.1
Iodine number g I.100 g 1 85 52 115
a
Measured at 25 °C.

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

Product 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
Corn oil – – – 10.6 0.1 – – 2.0 29.5 55.6 0.9 0.4 0.2 – – 0.2 0.2
Corn ME – – – 10.3 – – – 2.3 31.0 54.5 0.8 0.4 0.2 – – 0.2 0.2
Fleshing oil 3.1 1.4 0.4 26.0 6.5 0.9 0.9 11.4 45.8 2.5 0.3 – 0.3 – – – –
Fleshing ME 3.1 1.4 0.4 26.2 6.1 0.9 0.9 11.3 44.8 3.5 0.3 – 0.4 – – – –
Chicken fat 0.5 – – 19.8 3.8 0.4 – 6.1 34.6 30.9 2.9 – – 0.4 0.3 – –
Chicken ME 0.5 – – 19.4 3.6 0.4 – 6.1 32.2 32.8 2.9 – – 0.6 0.3 – –

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 final 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 alcohol–water–acid mix-
ture and the other phase mainly consists of the esterified 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 methanol–water–acid catalyst phase was removed by
settling, the ester–oil 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 per-
formed manually. First, the ester–oil mixture was subjected to a
heating at 65–70 °C to remove any remaining methanol for
20–30 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 first pretreatment.
After decreasing the FFA level of the feedstock below 1%, transe-
sterification reaction was completed with alkaline catalysts for the
fleshing oil and chicken fat. Because of the low FFA level of corn oil,
 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154
it was directly used in transesterification reaction to produce bio-
diesel. For transesterification reactions, potassium hydroxide and
methanol were used. The transesterification processes were the
same as those of pretreatment experiments except for catalyst.
After the transesterification reaction, the reaction mixture trans-
ferred 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 filtered
with 10-micron filter.
2.2. Characterization of fuel properties
The feedstocks and methyl esters were characterized in Alterna-
tive Fuels Research and Development Center in Kocaeli University
(AFRDC) and Marmara Research Center – The Scientific and Tech-
nological 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), flash 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 filter 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 composi-
tion (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,
fleshing 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%,
transesterification reaction was completed with alkaline catalysts.
On the other hand, the corn oil methyl ester was produced by
transesterification due to having low content of FFA. Fuel proper-
ties 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
transesterification reaction. The ingredient amounts used in the
transesterification 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 reac-
tion 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
transesterification. After transesterification and purification
process, the ester yield was found to be 91% on mass. This value
is slightly lower than the value obtained in the laboratory
2149
experiments. The reason for this may be higher amount of oil
and ester loss in the biodiesel pilot plant.
3.2. Biodiesel production from fleshing oil
In the previous study (Alptekin et al., 2012), optimum reaction
parameters were investigated to produce biodiesel from fleshing
oil in laboratory scale apparatus. Acid value of the fleshing 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
fleshing oil used in this study was 24.7 mg KOH g 1. The pretreat-
ment reaction parameters determined in the laboratory experi-
ments were used in pilot scale biodiesel production because the
properties of the fleshing oil used in the laboratory experiments
were very close to those of the fleshing oil used in this study.
The pretreatment conditions for fleshing oil were 30:1 alcohol
molar ratio and 10% sulfuric acid based on FFA level of the fleshing
oil. In the calculations, the molecular weight of the FFA was calcu-
lated to be the average molecular weight of the fatty acids in the
fleshing oil. The esterification process was repeated for two times
for the fleshing oil. The ingredient amounts used in the pretreat-
ment reactions for the fleshing oil were given in Table 3a.
The acid value of the fleshing 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 pro-
cess, there was oil loss about five percent of the fleshing oil during
the alcohol-catalyst-water removing and drying process. In addi-
tion to acid value, some properties of the pretreated fleshing oil
were characterized to understand the effects of pretreatment.
The pretreatment results were given in Table 3b. The density of
the fleshing oil and pretreated fleshing oil was measured at 25 °C
because they were in solid form at room temperature. The viscos-
ity, density and water content of the fleshing oil reduced after the
pretreatment reaction. The fuel properties of the pretreated oils
were very close to each other. This situation shows the repeatabil-
ity of the experiments. In this study, the sulfur content of fleshing
oil was above 990 ppm which is the maximum measurement value
of the sulfur analyzer. The reason of high sulfur content of the
fleshing oil is the results of the industrial process of the solid
wastes recycle plant where the fleshing oil was obtained. This
means that sulfur content of the feedstock is important to get
low sulfur content biodiesel after transesterification.
After pretreatment reactions, the FFA level of the fleshing oil
was 0.95% on average. The transesterification reaction parameters
were selected according to the previous study (Alptekin et al.,
2012). The ingredient amounts used in the transesterification reac-
tions for the fleshing oil were given in Table 3. The catalyst amount
was 1% weight of the initial amount of fat in the fleshing oil.
Additionally, neutralization amount was used which was calcu-
lated 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 fleshing oil for the transesterification
Table 3a
Ingredient amounts used in the pretreatment and transesterification reactions of the
fleshing oil.
Experiment 1 Experiment 2
Oil Alcohol Catalyst Oil Alcohol Catalyst
Pretreatment (kg) 50 21.1 0.62 50 21.1 0.62
Transesterification 45 11.3 0.4 + 0.1a 45 11.3 0.4 + 0.1a
(kg)
a
Neutralization amount.
2150 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154
Table 3b
Pretreatment results of the fleshing oil.
Property Unit
3
Density (25 °C) kg m
Viscosity (40 °C) mm2 s 1
1
Acid Value mg KOH g
Heat of Combustion kJ kg 1
Sulfur Content ppm
Water Content ppm
reaction. Mean molecular weight of the fleshing oil was found to be
about 850 g mol 1. After transesterification, the ester yield was
about 82% on average. Ester yield was calculated by dividing the
ester amount to the pretreated fat amount used for transesterifica-
tion. Transesterification results were given in Table 3c. The fuel
properties of the fleshing oil methyl ester were very close to each
other and fit 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 pretreat-
ment 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 corre-
sponds to FFA level of about 26.15%. Therefore, for this study, sev-
eral 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 first pretreatment
reaction. The reaction conditions were 1 h and 60 °C for the first
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 esterification 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 transesterification. In
addition, there was almost no difference between methanol molar
ratio of 30:1 and 40:1 with 20% sulfuric acid catalyzed pretreat-
ments. 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
Transesterification results of the fleshing oil.
Property Unit Experiment 1
Ester yield % mass 81.6
Density (15 °C) kg m 3 876.7
Viscosity (40 °C) mm2 s 1 4.69
Acid value mg KOH g 1
0.27
Heat of combustion kJ kg 1 39,917
Flash point °C 168
Fleshing Oil Experiment 1 Experiment 2
907.6 901.1 900.3
51.3 22.98 23.15
24.7 1.906 1.900
39,613 39,415 39,352
>990 >990 >990
2650 629 770
sulfuric acid and methanol molar ratio of 30:1 for 1 h at 60 °C
was thought to be sufficient for the first pretreatment reaction to
get high ester yield after transesterification. Thus, these reaction
parameters were selected for the first 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 transesterification
reaction. Therefore, these reaction parameters were selected for
the second pretreatment reaction.
The pretreatment reaction parameters determined in the labora-
tory 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 first pretreatment reac-
tion 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 first 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 dry-
ing process for the first and second pretreatment reactions, respec-
tively. The pretreated chicken fat was subjected to the second
pretreatment reaction. The esterification 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 first 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 alcohol–water–acid catalyst
removing process after pretreatment is very important to get low
sulfur content pretreated chicken fat. However, the second pre-
treatment results showed that there was no significant change in
Experiment 2
the sulfur content values after the first and second pretreatments.
82.3
Probably, some amount of sulfur cannot be separated with the
876.6
4.71
alcohol–water–acid catalyst phase and still it is included in the
0.30 ester-initial triglyceride phase. As will be stated in the next section,
39,849 the sulfur content of the pretreated chicken fat was decreased to
168 lower values by transesterification reaction.
 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154 2151

Table 4a
Ingredient amounts used in the pretreatment and transesterification reactions of the chicken fat.

Experiment 1 Experiment 2
Oil Alcohol Catalyst Oil Alcohol Catalyst
1st Pretreatment (kg) 45 40.5 2.4 45 40.5 2.4
2nd Pretreatment (kg) 40 3.1 0.1 40 3.1 0.1
Transesterification (kg) 35 6 0.27 + 0.08a 35 6 0.27 + 0.08a
a
Neutralization amount.

Table 4b
Pretreatment results of the chicken fat.

Experiment 1 Experiment 2
Property Unit Chicken fat 1st PT 2nd PTa 1st PTa 2nd PTa
3
Density (15 °C) kg m 937.6 914.2 912.2 915.4 911.6
Viscosity (40 °C) mm2 s 1 53.81 17.71 15.54 18.26 14.89
1
Acid value mg KOH g 52.30 3.36 1.93 3.32 1.95
Heat of combustion kJ kg 1 38,375 39,242 39,368 39,271 39,321
Sulfur content ppm 135 727 749 668 698
Water content ppm 4320 757 746 788 689
a
PT: pretreatment.

After two stage pretreatment reactions applied to chicken fat,
the FFA level was reduced to 0.97% on average. In the transesteri-
fication reactions, reaction parameters were chosen considering
the results in the previous study (Alptekin and Canakci, 2011).
The ingredient amounts used in the transesterification reactions
for the chicken fat were shown in Table 4a. The transesterification
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
transesterification and purification process, the ester yield was
found to be about 81% on average. The transesterification 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 transesterification reactions, two different methyl esters
were obtained for fleshing oil and chicken fat. Hence, these methyl
esters were mixed separately. Then, the fuel properties of all pro-
duced 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 specifications 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 param-
eters 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 876.7–889.7 kg m 3 which were suitable
Table 4c
Transesterification results of the chicken fat.
Property Unit Experiment 1
Ester yield % mass 80.4
Density (15 °C) kg m 3 889.6
Viscosity (40 °C) mm2 s 1 5.27
1 and FOME were 0.21, 0.28 and 0.43 mg KOH g 1, respectively.
Acid value mg KOH g 0.40
Heat of combustion kJ kg 1 39,728
Flash point °C 168
to biodiesel standards. Some of the physical properties limit the
use of biodiesel in diesel engines, especially viscosity (Encinar
et al., 2005). Viscosity influences 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 biodie-
sel 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
specified limit.
After transesterification, the ester may contain some unreacted
material such as triglyceride, residual alcohol, and residual cata-
lyst. Beside, traces of glycerol which is separated from biodiesel
in the production process can also be found in the final 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 transesterification is a
stepwise process, monoglyceride and diglyceride formed as inter-
mediates can also be found in biodiesel (Knothe, 2006; Çetinkaya
and Karaosmanoğlu, 2004; Tyson, 2001). These parameters give
information about the purity of biodiesels. The glyceride values
of the produced methyl esters were very low and fitted the biodie-
sel standards. The excess methanol used in the biodiesel produc-
tion process must be removed. The allowable methanol content
level is specified in biodiesel standards as 0.2%. The methanol con-
tents of the CFME, fleshing 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 flash point
being higher than that of diesel fuel. The flash points of the pro-
duced 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
Experiment 2 in the fuel which has influence on fuel aging. The EN 14214 and
81.5 ASTM D6751 have specified a maximum acid value of
889.8 0.5 mg KOH g 1 for biodiesel. The acid values of the COME, CFME
5.34
0.46
39,646 The copper strip corrosion is used for the detection of the corro-
169 siveness to copper of biodiesel fuels. The copper strip corrosion
2152 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154

Table 5
Fuel properties of the produced methyl esters.
1 2 3
Property Unit EN 14214 ASTM D6751-12 FOME FOME CFME CFME COME COME
3
Density (at 15 °C) kg m 860–900 – 876.7 875.5 889.7 883.0 886.0 884.0
Viscosity (at 40 °C) mm2 s 1 3.5–5.0 1.9–6.0 4.7 4.77 5.3 4.94 4.6 4.18
Flash point °C 101 min 130 min 168 175 169 172 169 192
Water content ppm 500 max – 410 326 440 NMa 440 NMa
1
Acid number mg KOH g 0.50 max 0.50 max 0.28 0.32 0.43 0.22 0.21 0.17
Monoglycerides % (mass) 0.80 max 0.40 max 0.06 0.27 0.02 0.56 0.06 NMa
Diglycerides % (mass) 0.20 max – 0.02 0.09 0.05 0.09 0.17 NMa
Triglycerides % (mass) 0.20 max – 0.20 0.04 0.06 0.12 0.06 NMa
Free glycerin % (mass) 0.02 max 0.02 max 0.01 0.01 0.008 0.02 0.01 0.013
Total glycerin % (mass) 0.25 max 0.24 max 0.05 0.10 0.03 0.19 0.06 0.17
Copper corrosion (3 h, at 50 °C) Degree of corrosion No 1 max No 3 max No 1 No 1 No 1 No 1 No 1 NMa
Heat of Combustion kJ kg 1 – – 39,892 39,954 39,693 40,173 39,878 NMa
Cetane Number – 51 min 47 min 58.8 NMa 52.3 NMa 54.2 NMa
Methanol content % (mass) 0.20 max 0.20 max 0.01 0.01 0.05 0.01 0.03 NMa
Sulfur content mg kg 1 10 max S15–15 max S500–500 max 138.1 141 81.5 NMa 4.1 NMa
Iodine value g I.100 g 1 120 max – 53.6 61 95.5 NMa 119.3 NMa
CFPP °C – – 10 11 3 2 5 1
a
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 pro-
duced methyl esters were not added to Table 5. Because, the oxida-
tion stability of the methyl esters were determined according to
PetroOXY’s Rapid Small Scale Oxidation Test (RSSOT) ASTM
D7545 method which has been approved but not incorporated into
ASTM fuel quality specifications. However, the oxidation stability
of COME, CFME and FOME were about 0.11, 0.12 and 0.2 h respec-
tively. On the other hand, the oxidation stability of diesel fuel was
about 1.5–2 h. The cetane number of a fuel shows the tendency of
that to self-ignite. Minimum cetane number of biodiesel is identi-
fied in ASTM D6751 as 47 while it is identified in EN 14214 as 51.
The cetane numbers of the produced methyl esters fulfilled 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 pro-
duced 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 confirmed 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 veg-
etable oil or animal fat. The iodine value is not listed in ASTM
D6751 while it is listed in EN 14214 biodiesel standard to be max-
imum 120. The iodine value of the produced methyl esters fitted
the biodiesel fuel standard value. The cold filter plugging point
(CFPP) is used to characterize the cold flow 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 com-
pared 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 depos-
its. 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 stan-
dard 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) 1182
Chicken fat (ton) 338
Fleshing oil (ton) 338
Methanol (ton) 2973
Sulfuric acid (ton) 1689
Potassium hydroxide (ton) 6419
Electrical (MW h) 84
Water (ton) 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 pro-
teins. In this study, as seen in Table 1, the sulfur content of the
fleshing 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 fleshing oil results
from the industrial process of the solid wastes recycle plant where
the fleshing oil was obtained because sulfuric acid is used in the
fleshing oil production. After the first pretreatment, the sulfur con-
tent of the chicken fat was increased. However, the sulfur content
of the pretreated chicken did not increase significantly 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, respec-
tively. The sulfur content of the animal fat methyl esters fitted
the ASTM D6751 (S500) biodiesel standard while they were not
suitable to EN 14214 biodiesel standard. The reason of the high sul-
fur content of these esters may be the sulfuric acid usage in the
biodiesel production. However, in some studies (Çolak et al.,
2005; Rashid et al., 2009), the sulfur content of the vegetable oil
or animal fat methyl esters did not fit 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 biodie-
sel 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 refining process in the biodiesel pilot
plant. In addition, another reason may be that the fuel properties of
 E. Alptekin et al. / Waste Management 34 (2014) 2146–2154
Table 6b
The biodiesel production costs for each feedstock.
Type of methyl ester Total cost (€/l) Methanol (€) Electricity (€)
Chicken fat 1.40 5383 273
Fleshing 1.13 5511 219
Corn oil 1.62 3924 168
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 mar-
ket feasibility of biodiesel. In this study, low cost feedstocks such as
chicken fat and fleshing 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 oper-
ating 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 transesterification
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 transesterification reactions were recov-
ered. 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 coun-
try due to the currency difference. Therefore, it should be noted
that the final 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, electric-
ity 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 fleshing oil for pretreat-
ment reactions as seen in Table 6b. Using higher amount of cata-
lysts increases the price of CFME. This means that the FFA level
of the feedstock directly influences the biodiesel cost. The opera-
tion cost of CFME is the lowest. However, it was still more expen-
sive 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 fleshing 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 significant differences in the fuel proper-
ties of methyl esters between laboratory and pilot plant experi-
ments. Methyl esters produced in the laboratory and pilot plant
experiments showed similar properties. One or two step acid cata-
lyzed 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 transesterifica-
tion reactions resulted in good ester yields. Ester yield value of
2153
Water (€) Base catalyst (€) Acid catalyst (€) Feedstock (€)
44 532 938 3380
51 678 209 3380
60 642 – 11,820
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 flow 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 flow properties of the FOME should
be improved with cold flow enhancers or it may be mixed with
petroleum diesel fuel which has better cold flow properties. Exper-
imental results showed that the sulfur content of the biodiesel
feedstock is very important to get low sulfur content biodiesel after
transesterification. The sulfur content of COME was much lower
than those of animal fat methyl esters. On the other hand, the first
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. Never-
theless, the animal fat methyl esters fitted the ASTM D6751 (S500)
biodiesel fuel standards. According to the economic analysis, the
costs of biodiesels produced from corn oil, chicken fat and fleshing
oil were 1.62 €, 1.40 € and 1.13 €, respectively.
Acknowledgements
This study was supported by the grants from Scientific 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 Beypiliç Chicken
Slaughterhouse (Bolu) managements for supplying the feedstocks.
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