A COMPARISON OF COLD FLOW PROPERTIES OF BIODIESEL PRODUCED FROM

VIRGIN AND USED FRYING OIL

a b b c
Filiz Al-Shanableh , Ali Evcil ,Cemal Gövsa , Mahmut A. Savaş
a
Food Engineering Department, Near East University, Nicosia, NORTH CYPRUS
b
Mechanical Engineering Department, Near East University, Nicosia, NORTH CYPRUS
c
Mechanical Engineering Department, Boğaziçi University, Bebek, İstanbul, TURKEY

ABSTRACT
The cold flow properties of biodiesel produced from two types of feedstock, namely refined-virgin frying vegetable oil (RVFVO)
and waste frying vegetable oil (WFVO) were compared in this work. Biodiesel fuel derived from fat or oil which contains
significant amounts of saturated fatty compounds are known to display higher cloud points (CP), cold filter plugging points
(CFPP) and pour points (PP). Both RVFVO and WFVO were obtained from the same cafeteria in the Near East University
campus and converted to biodiesel fuel via base catalyzed transesterification reaction. The cold flow properties CP , CFPP and
PP were found as 15 °C, 13°C and 11 °C, respectively, for RVFVO and 15 °C, 14°C and 12 °C, respectively, for WFVO. The
current results show that the biodiesel produced from RVFVO and WFVO exhibit no considerable differences in their cold flow
properties. Hence, WFVO appears to have no drawbacks as a raw material in biodiesel production in addition to its lower cost
and also environmental benefits.

Keywords: biodiesel, refined virgin vegetable oil, waste frying vegetable oil, cloud point, pour point, cold filter
plugging point

INTRODUCTION

The World’s major concern in the energy production is the protection of environment and the conservation of non-
renewable energy resources. This requires alternative development of the sources of energy as substitutes of
traditional fossil fuels. The alternatives to diesel fuel for instance must be technically feasible, economically
competitive, environmentally acceptable, and readily available. In liquid fuels, biodiesel is one of the most popular
alternatives due to its suitability for the conventional diesel engines with minimum or no modifications, as well as in
blends with petroleum diesel. Biodiesel can be derived from the renewable lipids (triglycerides) feedstock
(vegetable or animal oils/fats). Despite numerous of its benefits biodiesel has recently received substantial bad
press (Karasu 2011, Smith and Elliot 2008). These criticisms are based primarily on the use of scarce food and
agricultural resources as feedstock. In the Turkish Republic of Northern Cyprus (North Cyprus), about 5 million
liters (4.5 thousand tons) of vegetable oils (mainly sunflower oil) is consumed every year as food products (State
Planning Organization Report, 2008) of which almost all is imported from abroad and 1.2 million liters
(1.1 thousand tons) of waste frying oil is produced each year. However a very small portion of the waste frying oil
has been reclaimed and reused. Until now the waste frying oil is often flushed down the drains. In such a heavy
dependence of oil/fat resources, their waste can be utilized as an alternative raw material for biodiesel production.
Conversion of waste frying oil to biodiesel is not only expected to reduce engine exhaust gas pollution, but also
can replace food-derived fuels and reduce ecologic water pollution. Two types of vegetable oil feedstock for
biodiesel production searched in this project were Waste Frying Vegetable Oil (WFVO) and Refined-Virgin Frying
Vegetable Oil (RVFVO).

Biodiesel has been traditionally derived mainly from virgin vegetable oil that is a renewable source (Shahid and
Jamal 2008, Öğüt and Oğuz 2006, Acaroğlu 2007, Uluengin 2007, Balat and Balat 2008,Sharma et al 2007,
Steinbach 2008). The use of biodiesel is almost as old as the diesel engine itself. Rudolf Diesel patented his
engine in 1892 that could run on peanut oil (Shahid and Jamal 2008). After 1940’s huge reservoirs of petroleum
were discovered and diesel fuel produced from petroleum became cheaper than biodiesel. Nevertheless, the
situation has changed recently due to a number of reasons. The petroleum reserves will last for a limited period of
time. Biodiesel fuel from a domestic source reduces the petroleum imports of a country. It is a fuel also with lower
exhaust emissions. Carbon dioxide released by combustion of biodiesel can be recycled by photosynthesis which
minimizes the green house effect (Zhang et al 2003). Biodiesel has a flash point (~150°C) higher than that of
petroleum diesel (~77°C) therefore, less volatile and safer to transport. It has a lower volumetric heating value but
has a high cetane number. It provides lubricating properties that reduces engine wear and extend engine life.
The earliest diesel motors had large injectors since they used viscous vegetable fuel. Then, due to the low
petroleum prices the engine technology was adjusted to consume the low viscosity petroleum diesel. The
vegetable oil is demanded again at present as it was in the early diesel engines, however, their high viscosity is
not suitable for the current diesel vehicles. The high viscosity results in poor atomization, incomplete combustion
and carbon deposition on the injector and the valve seats, causing serious engine contamination (Sharma et al
2007). Other drawbacks of the direct use of vegetable oil include low volatility and polyunsaturated character.
Nevertheless, since 1970’s a low viscosity biodiesel can be produced by processing the vegetable oil using
processes like pyrolysis, micro-emulsification or transesterification. In the transesterification (or alcoholysis)
reaction which is catalyzed by a base, acid or enzyme, a virgin vegetable oil, WFVO or animal fat is reacted with
an alcohol to yield fatty acid methyl esters (FAME), i.e. biodiesel, and a glycerol co-product which has a
commercial value. Among these options, the base catalyzed transesterification (Encinar et al 2007, Steinbach
2007) is considered to be the most promising route for lowering viscosity. During the transesterification reaction,
triacylglycerol reacts with methanol allowing the three fatty acid chains to be released from glycerol skeleton and
combine with alcohol to yield fatty acid methyl esters and glycerol as shown in Fig. 1.

Fig. 1. A Schematic representation of the transesterification of triacylglycerol with methanol to yield FAME (biodiesel fuel) and glycerol using base
catalyst.

At present, the main oilseeds used in extracting vegetable oil are mostly sunflower and rapeseed seeds in Turkey
(Öğüt and Oğuz 2006) and Greece (Panoutsou et al 2008), and soybean seeds in US (Zhang et al 2003). The cost
of biodiesel produced from virgin vegetable oil is about 1.5 times of the petroleum based diesel. Virgin vegetable
oil makes-up about 75% of the total cost of biodiesel production (Phan and Phan 2008, Öğüt and Oğuz 2006). The
production of biodiesel from vegetable oil has debated also due the use of fertile land to crop oilseeds which
reduces the land available for food crops. The result is an increase in food prices and making food scarce all
around the world. Hence, the use of waste vegetable oil instead of virgin vegetable oil is desirable to reduce not
only the raw material cost but also in terms of a number of environmental issues. The cost of waste oil is estimated
to be less than half the price of virgin oil (Encinar et al 2007), e.g. reported as US$ 0.22 per liter in Brasil (Araujo et
al 2010) and is still free in NORTH CYPRUS. In addition, the utilization of WFVO reduces the environmental
pollution. On the other side, WFVO has properties different from those of petroleum products and RVFVO. The
high temperatures of cooking procedures and the water from the foods rapidly hydrolyze the triglycerides and
increase the free fatty acid content in the oil. The undesirable free fatty acid (FFA) content increases with the frying
time. Other drawbacks such as the stability of mixtures, variations in viscosity, iodine value, density, optimization
of methanol consumption have to be taken into consideration. To summarize, WFVO seems to be a lower quality
raw material as compared to RVFVO in biodiesel production.

Growth of population and increasing food consumption have increased accumulation of WFVO from households,
restaurants, hotels, schools and industrial sources. This is a growing problem not only in North Cyprus but also all
around the world. Being an island, the situation appears to be more serious in Cyprus as compared to the
mainland. The WFVO poured down the sinks and drains, causes problems for sewage treatment plants increasing
the depuration costs. The municipalities often collect WFVO from schools, restaurants, hotels and industrial
sources then, dump it into a waste disposal area without sewage treatment. This poses a detrimental
environmental effect on soil, rivers and sea, and eventually on the living matter. An example of such a waste
disposal area in the north of Nicosia is located only a few kilometers away from the Near East University. The
municipalities and the government often have been criticized in daily newspapers for not keeping their words in
improving waste treatment (Eminoğlu 2010). In fact, WFVO is a valuable residue and can be considered as a
potential raw material for soap manufacturing, energy production by means of anaerobic digestion, thermal
cracking and more recently for biodiesel fuel production (Phan and Phan 2008, Sabudak and Yıldız 2010, Araujo
et al 2010, Zhang et al 2003, Encinar et al 2007, Maceiras et al 2009). The European Parliament banned the use
of WFVO in the manufacture of animal food in 2004. The same ban has been in effect in Turkey since 2005.
Hence, WFVO can be utilized as a raw material primarily in biodiesel production. Although it is a valuable waste
and a major raw material for biodiesel production, there are no major organizations either, private (Araujo et al
2010) or state (Uluengin 2007) that collect WFVO in North Cyprus. The result of an informal survey, given in
Fig. 2, in prior to the experimental work revealed that the university cafeterias can be a major source of WFVO.
The smallest amount of WFVO is accumulated in kebab houses. While about 85 % of the RVFVO could be
recovered as WFVO in the university campus and in fast food restaurants, this value drops to 25 % for kebap
houses. As a result, on average 67 % of vegetable oil/fat that was consumed could be recovered as WFVO from
the typical food establishment in North Cyprus.

1000
900
RVFVO versus WFVO ( L / week)

800
700
600
500
RVFVO
400
WFVO
300
200
100
0
University Restaurant Fast Food Hotel Kebap
Cafeteria Restaurant House

Fig. 2. Average accumulation of RVFVO and WFVO in liters per week for typical food establishments in North Cyprus.

Major biodiesel standards which serve as a reference for other standards are EN 14213:2003 (Heating Fuels) and
EN 14214:2003 (Automotive Fuels) or ASTM D6751-09. The tendency of a diesel fuel to gel or solidify at low
temperatures is well known. Biodiesel starts to gel at higher temperatures than diesel fuel and its cold flow
characteristics are rather poor. Determination of the cold flow characteristics and its improvement is a major
challenge. There are three important parameters for low temperature characteristics of biodiesel fuel, namely, CP
(cloud point), PP (pour point) and CFPP (cold filter plugging point). CP is the temperature at which cloud of wax
crystals first becomes visible when fuel is cooled under conditions described by ASTM D2500-09 or ISO
3015:1992. More sophisticated procedures have been published for cloud point measurement in recent ASTM
D3117-03, ASTM D5771-05, ASTM D5772-05 and ASTM D5773-07 standards. However, these are not essential
in ASTM D6751, yet. PP is the temperature at which the amount of wax crystallizes is sufficient to gel the fuel, thus
it is the lowest temperature at which fuel can flow. The sample must be cooled following the procedure described
either in ASTM D97-05 or ISO 3016:1994. CFPP is described in ASTM D6371-05 and EN 116:1998 and directly
affects the diesel engine performance in winter. It determines the lowest temperature where 20 ml of fuel can be
drawn through a 45 micron screen in 60 seconds with 200 mm of water (1.96 kPa) vacuum. CP is the highest
temperature used for characterizing cold flow and PP is the lowest. CFPP is usually between cloud and pour
points. Cloud point is a must in ASTM D6751 standard; pour and filter plugging points rather than cloud point are
listed in EN 14213 and EN 14214 standards.

EXPERIMENTAL METHOD

Biodisel Production From RVFVO and WFVO

The design of a biodiesel production installation can be based on its capacity (Öğüt and Oğuz 2006, Uluengin
2007). A large commercial scale installation is designed to produce between 200 - 1000 liters of biodiesel per
hour. A medium scale installation is capable of producing about 100 liters of biodiesel per hour. The laboratory
scale experimental set-up used in the current work was a 2 liters batch type installation for brewing biodiesel
samples. A flow chart of the experimental procedures followed (Bulun et al 2011) is shown in Fig. 3.

In the current study, biodiesel was produced from RVFVO and WVFO by means of base-catalyzed one-step
transesterification reaction. Properties featured by WVFO differ from those of RVFVO. The presence of heat and
water accelerates the hydrolysis of tri-glycerides and increases the free fatty acid (FFA) content. FFA and water
contents degrade the transesterification of glycerides with alcohols. They also interfere with the separation of fatty
acid esters and glycerol. Thus, triglycerides containing high amounts of water and FFA are not easily
transesterified. Hence, pretreatment of WVFO was necessary. Additional preprocesses such as filtration and water
removal were performed during biodiesel production.

During the production, three operations were performed namely, transesterification, phase separation and
purification. In this study, methanol was used and methyl esters were produced. After the reaction was completed,
the products were separated into two layers. The ester product floated to the top and the by-product glycerol
precipitated as the bottom layer. After the separation of ester product from the glycerol, the catalyst and alcohol
were washed from the methyl ester using water.

Fig. 3. Flow chart of the experimental procedures followed in the present study.

Collection and Pre-treatment of WVFO

As frying oil the RVFVO was used in the university cafeterias and its waste WVFO accumulated after two to three
days depending on the work load were collected. The RVFVO that has the trade name Cicekyag-Balıkesir is a
mixture of mainly palm oil which is imported from abroad, cotton seed oil, soybean oil and sunflower oil with major
fatty acid composition as seen in the Table 1. While RVFVO did not require any pretreatment, WVFO was filtered
to remove food residues and solid precipitates then, heated to 100 - 120°C to remove water before the
transesterification conversion. Percentage of solid particles was calculated after filtration. It was found that WVFO
contained about 2 % solid particles and also water between 4 - 5 %.
Table 1. Fatty acid composition of RVFVO (Cicekyag)
Major fatty acid composition
Palmitic acid Stearic acid Oleic acid Linoleic acid Others
C16:0 C18:0 C18:1 C18:2
Composition (wt %) 47 5 34 13 ~1
Molar mass (g/mol) 256.42 284.48 282.46 280.45
Density(g/cm3) 0.853 0.847 0.895 0.900

A high FFA content was undesirable in the transesterification process since higher the acidity of the sample of
vegetale oil lower the conversion to biodiesel fuel. Titration was necessary to determine the FFA content in
feedstocks otherwise, a part of the catalyst (NaOH) used in the process would be consumed to neutralize FFA and
this would affect the completion of reaction. FFA in the samples was found by titrating against NaOH and then the
amount of base catalyst (NaOH) necessary to neutralize FFA was calculated. The % FFA is usually used to
describe the FFA content of oils, while Acid Value (AV) is commonly used to describe the FFA content of finished
biodiesel. % FFA is defined as the percentage by weight of free acid groups found in an oil sample, while AV is
defined as the weight of KOH in mg required to neutralize. The Acid Value is one of the tests (ASTM D 664)
required for the final biodiesel product. % FFA can be calculated using Eqn.(1) and can be converted to AV using
Eqn.(2) (Wrolstad et al 2005) below.
(VNaOH )(NNaOH )(MWoleic acid )
% FFA as oleic acid = (1)
Weight of sample

where
VNaOH = Volume of NaOH consumed in titration
NNaOH = Normality of NaOH.
MWoleic acid = Molecular weight of oleic acid. (Most of FFA in vegetable oil was consider to be oleic acid)
Weight of sample = (Density of oil sample) x (Volume of oil sample)

𝑁𝐴 = (% 𝐹𝐹𝐴) × 1.9 (2)

% FFA calculated and converted into AV is listed in Table 2 .

Table 2: % FFA and AV of oil samples used in biodiesel production.

Type of oil used VNaOH % FFA Acid Value (AV)

RVFVO 0.8 mL 0.67 1.3

WVFO 1.3 mL 1.1 2.2

Transesterification Reaction

The transesterification reaction involved a chemical reaction between triglyceride and methanol in the presence of
NaOH as the catalyst. The high purity NaOH and methyl alcohol supplied by Merck were used as catalyst and
alcohol. Methanol to oil molar ratio was taken as 6:1 instead of 3:1 that means excess alcohol used to ensure
completion of transesterification reaction. The amount of NaOH in grams needed for 1 liter of RVFVO or WVFO
was determined using 1 wt % NaOH to accelerate the transesterification reaction plus mass of NaOH obtained
from titration that was consumed to neutralize RVFVO or WVFO (Bulun et al 2011, Shnaikat et al 2010). A 2.0 liter
three-neck flask was used as continuous stirring tank reactor (CSTR) that was equipped by magnetic stirrer and
heater as seen in Fig. 4(a). Reaction took place at atmospheric pressure and in the vicinity of 60oC for one hour.

Separation and Purification of Biodiesel

The resulting mixture obtained after the reaction was poured into a 2.0 liter separation funnel and kept minimum
eight hours for separation. The less dense ester was separated by gravity and floated to the upper section of the
funnel as seen in Fig. 4(b). The glycerol, excess methanol and undesired products were segregated to the bottom
of the separation funnel and were decanted. The upper layer was collected for further purification by washing.
Washing was a process to remove the entrained glycerol, catalyst, soap and excess methanol. Warm distilled
water was used for washing the biodiesel to avoid the contamination of oil. The clear water was settled at the
bottom of the separation funnel and biodiesel was formed at the top layer as seen in Fig. 4(c). Washing was
repeated until to obtain a pH level of 7.0 in the water separated.

(a) (b) (c)

Fig. 4. Laboratory scale biodiesel production: (a) Transesterification reactor, (b) Separation of crude biodiesel (FAME) from crude glycerol,
(c) Purification of FAME

Drying was ascertained by heating the washed fuel approximately to 110 oC in an open container. Heating was
carried out until no more water vapor came out of the fuel. The heating process also evaporated any traces of
remaining alcohol as well. Finally from highly viscous RVFVO and WFVO which were provided from the Near East
University cafeterias (Fig. 5(a)), the end products that is the final biodiesel were obtained which appeared as a
clear, amber-colored liquid as shown in Fig. 5(b).

(a) (b)
Fig. 5. From triglyceride to biodiesel: (a) WFVO (left) and RVFVO (right) obtained from the university campus cafeteria,
(b) Biodiesel produced from WFVO (left) and from RVFVO (right).

Determination of Cold Flow Properties

Cloud Point and Pour Point Set-up

The apparatus used for CP and PP measurements were manufactured following the ASTM and EN - ISO
standards (Gökçe and Kırmaz 2010, Al-Said and Nadeem 2010). A glass jar containing 45 ml biodiesel sample
was fitted into an aluminum cylinder that was placed in the middle of the apparatus shown schematically in Fig. 6.
It was important that the glass jar should be thermally insulated from the aluminum cylinder by means of a cork
disk, stopper and ring assembly. The assembly was inserted in an 8 liter stainless steel cooling bath containing
brine at -12 oC. The cooling bath itself was embedded in an 11 cm thick styrofoam (polystyrene) block to isolate it
against heat transfer and vibration. The entire assembly was secured in a 3 cm thick wooden box. It was noted
that the temperature of the cooling bath remained almost unchanged after 24 h. Temperature of the biodiesel
sample was measured using an ASTM 5C type thermometer then, repeated with a T-type thermocouple. The
biodiesel sample was cooled under those conditions described in the ASTM or ISO standards. Three
measurements were made for each sample to check the consistency of the data collected.
Fig. 6. Apparatus manufactured to determine the CP and PP temperatures

Cold Filter Plugging Point Set-up

Cloud point and pour point set-up was also used for CFPP measurements with the addition of a vacuum system
and a pipette with filter unit. The apparatus manufactured (Pervais et al 2010) was slightly deviated and also a
modified version of the system prescribed in ASTM D6371-05 and EN 116:1998. The double oblique bore
stopcock was replaced by three valves and named as (1) air flow rate adjusting valve, (2) suction valve and (3)
release valve. Air flow rate of the vacuum source was adapted to the required level, at 200 mm water of vacuum,
using the air flow rate adjusting valve. At the beginning of each test suction and release valves were closed and
the tests were started by opening the suction valve after placing the pipette with filter unit into the test jar. After
each test, the release valve was opened for the sample to drain back to the test jar.

Fig. 7. The mesh of the plastic filter used and the micron scale (top).

Two plastic filters were used together and each filter had a nominal aperture size of 160 μm and a nominal wire
diameter of 80 μm as can be measured from the micron scale placed on top of Fig. 7. Use of single and triple
filters resulted in lower and higher values of CFPP than expected. CFPP is normally expected to be between CP
and PP. However, only the double filter usage resulted in reasonable values of CFPP.

RESULTS AND DISCUSSION

Efficiency of Biodiesel Production

Transesterification was successfully employed in the experimental work to reduce the viscosity. Methanol, a less
expensive alcohol, was used during transesterification reaction. Sodium hydroxide was used in the production of
biodiesel due to its availability and also it reduces the production cost. The molar ratio of alcohol to oil was
calculated as 3:1 by stoichiometry, but excess methanol was added in ratio of 6:1 for a higher yield in a shorter
time. Average percent conversion of WVFO that was used to produce biodiesel could be estimated using the Eqn.
(3) (Phan et al 2008).
𝑚𝑒𝑠𝑡𝑒𝑟
% 𝐶𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛 = 𝑚𝑜𝑖𝑙 (3)
3× ×𝑀𝑊𝑒𝑠𝑡𝑒𝑟
𝑀𝑊𝑜𝑖𝑙

where mester is the weight of ester collected (g), moil is the weight of the oil sample (g), MWoil is the averaged
molecular weight of oil sample, MWester: averaged molecular weight of fatty acid ester.

𝑀𝑊𝑜𝑖𝑙 = 3 × ∑𝑖(𝑀𝑊𝑖 × % 𝑚𝑖 ) + 38 (4)

where; MWi: molecular weight of fatty acid i; %mi: percentage of fatty acid i in the raw material.

𝑀𝑊𝑒𝑠𝑡𝑒𝑟 = ∑𝑖(𝑀𝑊𝑖 × % 𝑚𝑖 ) + 14 (5)

Molar mass of RVFVO and molar mass of methyl ester produced from tranesterification reaction were calculated
using Table 1 as 848.3 g/mol and 284.1 g/mol, respectively. Molar masses of WVFVO and its methyl ester were
considered to be the same molar masses as RVFVO and its methyl ester. The percent conversion results are
shown in Table 3. Reason of decrease in conversion after purification process, is the mass lost during washing
and heating.

Table 3. % Conversion of RVFVO and WVFO to methyl ester.

Type of Oil % Conversion of % Conversion of FAME
used FAME produced after purification

RVFVO 98.3 89.0

WVFO 97.9 87.8

Cold Flow Characteristics of Biodiesel Produced

CP, PP and CFPP were measured for biodiesel produced from RVFVO and WFVO are shown in Table 4 together
with diesel 2 fuel (Acaroğlu, 2007). The cold flow characteristics of biodiesel produced can be considered as poor
when compared with diesel 2 fuel. All three temperatures were higher than their counterparts given for the diesel 2
fuel and also the biodiesel produced from other type of vegetable oils and their wastes (Tang et al.,2008, Encinar
et al., 2006). This behavior is attributed primarily on the large amounts of saturated fatty compounds present in oil
samples and high content of palmitic acid portions. Udomsup et al showed that high content of palmitic acid (that is
63 wt % for their work) in palm stearin methyl ester was caused extremely increase in CP and PP values as
reported as 18oC and 19.4oC respectively.

Table 4. Cold flow characteristics of the biodiesel produced from RVFVO and WFVO.
Test Methods Cold Flow Properties (oC)
Biodiesel Biodiesel Biodiesel
Property EN 14214/14213 ASTM D6751 produced from produced from Diesel 2 Fuel
RVFVO WFVO
CP ISO 3015:92 ASTM D2500-09 15 15 -16
PP ISO 3016:1994 ASTM D97-05 11 12 -27
CFPP EN 116:1998 ASTM D6371-05 13 14 -18

Once CP is determined as 15oC for both biodiesel samples produced from RVFVO and WFVO, the CFPP can be
estimated as 12.4oC by employing the empirical relation (Acaroğlu, 2007) below before an experimental
measurement.

𝐶𝐹𝑃𝑃 = 1.019 (𝐶𝑃) − 2.9 (6)

Considering that the error in temperature measurements is ±1.5oC (ASTM D2500-09) the CFPP values estimated
can be regarded as good assessments since they differ only about 5 % and 11 % for biodiesel samples produced
from RVFVO and WFVO, respectively. ASTM D6751 specifies the maximum CFPP temperatures as 0 oC between
April 15 and September 30, -10oC from October 1 to November 15, -20oC between November 16 – February 28
and -10oC from March 1 to April 14 in the US.

The monthly average minimum climatic temperatures obtained from Meteorology Department of North Cyprus can
be seen in Fig. 8. The lowest average minimum temperatures were observed as 5o C during January and
February. Not only CFPP but also PP and CP temperatures of the biodiesel produced from RVFVO and WFVO
were above 5 oC. It appears that the pure biodiesel can be suitable from May to October, i.e. in the six months of
the year in Nicosia. Nevertheless, a common remedy to lower cold flow temperatures including CFPP is to blend
commercial diesel fuel into the biodiesel.

25

20
Ave. Min. Temp. (ºC)

15

10

0
J F M A M J J A S O N D
Months

Fig. 8. Monthly average minimum temperatures in Nicosia during a year.

Modifications Made in the CP and CFPP Measurement Set-Ups

The test procedure to measure CP both in ASTM D2500-09 and ISO 3015:1992 has been criticized particularly, by
the oil companies (Kruka and Cadena 1995) because it may contain some inaccuracies. In an attempt to measure
CP more accurately the following measures were taken in the present work.

(i) The cloudness is assessed by visual examination close to the flat bottom end of cylindrical test jar of
approximately 34 mm in diameter and 120 mm height in the two standards. The visual examination is
subjective and may lead to variations both in temperature readings and also in the definition and size of the
cloud formed in the biodiesel. After the preliminary tests, the use of a magnifying glass was found to be helpful
in observing the cloud formation and also the temperature reading.

(ii) A second source of inaccuracy was the delay in temperature reading from the thermometer since a short but a
finite time was necessary. An additional time was spent when the thermometer was taken out of the test jar for
temperature reading in the vicinity of cloud point. The thermometer temperature would rise in that time interval.
There would also be a delay in reading the actual CP temperature as a result of the thermal inertia of mercury
thermometer. Following the measurement of CP using a thermometer, the employment of a T- type
thermocouple allowed checking any discrepancy in temperature reading.

ASTM D2500 has been blamed by the oil companies because the test procedure for cloud point determination is
not applicable to dark crude oils and also does not account for potential undercooking of the wax. Absence of
stirring can be another problem. Kruka and Cadena reported that stirring and use of a rapidly responding
thermocouple gave a slightly higher cloud point than ASTM D2500 procedure. They argued that the actual cloud
point would be somewhere between the average of the heating and cooling cycle cloud points and the heating
cycle value. In this context, a cooling curve test such as described in ASTM D87-09 can be beneficial in measuring
of CP precisely. Alternative and more sophisticated test methods have been published by ASTM (ASTM D3117-
03, ASTM D5771-05, ASTM D5772-05,ASTM D5773-07). Nevertheless, the procedure described in the current
ASTM 2500 and ISO 3015 is the official test method required to measure CP.
The exact measurement of CP is critical since it precedes CFPP. The wax crystals stick together to form bigger
ones below CP then, these larger crystals block fuel filters and plug fuel lines when CFPP is reached. It can be
argued that the error involved among the three temperatures measured may be the smallest in PP measurement.

CONCLUSIONS

The use of WVFO instead of RVFVO to produce biodiesel is an effective way to reduce the raw material cost.
Using WVFO also helps to relieve the problem of waste oil disposal. The results of an informal survey revealed
that the university cafeterias were the highest source of WVFO whereas the lowest amount of WVFO was
accumulated in the kebab houses. The biodiesel of the current survey was produced from RVFVO and WVFO
using a transesterification reaction. The average percent conversion of RVFVO and WVFO to biodiesel was 98.3
% and 97.9 % respectively, and dropped to 89 % and 87.8 % following purification. The biodiesel produced from
RVFVO and WVFO was waxed at a higher temperature than the commercial diesel fuel and also the biodiesel
obtained from most virgin vegetable oils because of high palmitic and oleic acid contents of frying oil. The three
important parameters for low temperature applications, i.e. CP, PP and CFPP were found as 15 oC, 11oC and
13oC, respectively for RVFVO and 15°C, 14°C and 12°C, respectively, for WFVO following the current ASTM and
EN standards . Results showed that the biodiesel produced from RVFVO and WFVO exhibit no considerable
differences in their cold flow characteristics. The poor cold flow characteristics limit the use of pure biodiesel from
May to October in Nicosia. Nevertheless, all three properties can be improved when the biodiesel is blended with
commercial diesel fuel thus; allowing proper blends for the winter season.

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