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Preparation and evaluation of biodiesel from Egyptian castor oil from

semi-treated industrial wastewater
Nabel A. Negm a,∗, Magdy A. Shaalan b, Gamal S. El Barouty b, Mona Y. Mohamed a
a
Petrochemicals Department, Egyptian Petroleum Research Institute, Nasr City, P.B. 11727, Cairo, Egypt
b
Faculty of Agriculture, Cairo University, Giza, EGYPT

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

Article history: Biodiesel derived from Egyptian castor oil was prepared via the conventional base-catalyzed transesteri-
Received 6 November 2015 fication with methanol. Fatty acid profiles of castor oil and the obtained fuel properties of the biodiesel
Revised 13 February 2016
were analyzed and tested in accordance with the ASTM standards. Castor oil contains: > 6%, > 6%, > 8%,
Accepted 18 February 2016
82% of saturated, monounsaturated, polyunsaturated and hydroxy mono-saturated fatty acids, respec-
Available online xxx
tively. The present study reports the preparation of biodiesel from castor oil using sodium methoxide
Keywords: as a catalyst. The resultant biodiesel was evaluated for physic-chemical properties namely: Iodine value
Castor oil (82.7 g I2 /100 g oil), cetane number (55.82), density (0.878 g/cm3 ), kinematic viscosity (40°C: 4.65 cSt;
Transesterification 100°C: 1.28 cSt), cloud point (0 °C), flash point (151 °C), fire point (156 °C), carbon residue (0.052 %), and
Biodiesel ash residual (0.025%). The obtained biodiesel properties were compared with those of several biodiesels
Fuel properties from different vegetable oils such as: sunflower, soybean and rapeseed oils and found to be compara-
Engine test
ble. The performance of the diesel engine was improved by blending regular diesel with 10 % biodiesel
(B10). The brake specific fuel consumption was decreased using B10 blend. The brake thermal efficiency
was also increased for B10 from 25% to 27.36%. The brake specific fuel consumption was increased for B10
blend compared to regular diesel. In general, Egyptian castor oil has been identified as the ideal feedstock
for biodiesel production, and was found to be the promising feed stock for biodiesel production.
© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction esters (FAMEs) used as biodiesels are biodegradable and non-toxic

Conventional fossil-based fuels are not renewable and are des-
tined to become exhausted, which inspires the use of alternative
fuels [1]. Recently, global warming due to the heavy consumption
of fossil fuels and the depletion of natural resources has become
an increasing cause of concern. For the considerations of sustain-
able development, biomass –to-biodiesel has progressively gained
international attention as a potential source of renewable energy.
Biodiesel is a mixture of fatty acid methyl esters (FAME) obtained
from plant seed oil by the transesterification reaction. This reac-
tion occurs after heating the triglycerides in plant seed oil with
methanol in the presence of a catalyst, with the resulting prod-
uct mixture comprising FAME and glycerol. The homogeneous cat-
alyst system transesterification reaction is relatively fast with high
conversion [2]. Biodiesel has received increasing attention due to
its less polluting nature and because it is a renewable energy re-
source as opposed to conventional diesel [3]. Fatty acid methyl
∗
Corresponding author. Tel.: +20 2 22745902; fax: +20 2 22747433.
E-mail address: nabelnegm@hotmail.com (N.A. Negm).
to plants, animals and humans. These biodiesels can be mixed with
petroleum diesel in any proportion or directly used in diesel en-
gine without modification [4]. The high cost of biodiesel is the
major barrier to its commercialization [5], and 80 % of the to-
tal cost of biodiesel production is the cost of the raw materi-
als [6]. The choice of feedstock for today’s commercial biodiesel
plants depend largely on geography; rapeseed oil dominating the
EU production, soybean oil dominating the US and Latin Ameri-
can production, and palm oil mainly being used in Asia. There is
an increasing interest to search for suitable alternative oils for the
production of biodiesel [7, 8] as the use of edible oils are being
discouraged globally. Even though several non-edible oils like Ja-
tropha and karanja are being exploited for biodiesel preparation,
very few unusual fatty acids-containing oils such as castor oil and
lesquerella have been exploited for this purpose. Studies on cas-
tor oil and lesquerella suggested that their uniquely high level of
the hydroxy fatty acids which impart increased lubricity to the oil
and its derivatives as compared to other vegetable oils [9]. Bio-
fuels are obtained by cracking of different vegetable oils includ-
ing: Alcea pallid oil [10], woody oils [11], soybean oil [12], palm
oil [13], cotton seeds oil [14], Jatropha oil [15], and waste cooking

http://dx.doi.org/10.1016/j.jtice.2016.02.024
1876-1070/© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Please cite this article as: N.A. Negm et al., Preparation and evaluation of biodiesel from Egyptian castor oil from semi-treated industrial
wastewater, Journal of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.02.024
JID: JTICE
ARTICLE IN PRESS
2 N.A. Negm et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–6
oils [16]. Cracking oil vegetable oils performed either thermally
without using any type of catalyst [17], or by using alkaline cat-
alysts [18], metal oxides [19], zeolite [20–22]. Fish oils [23], ani-
mal fats [24] and microalgae oils [25] are also used as consider-
able sources for biofuels. Owing to economic reasons, the use of
low cost raw material, such as Egyptian castor oil (ECO) planted in
Upper Egypt in Al-Alaki valley and irrigated using industrial and
pretreated wastewater, is being considered for biodiesel produc-
tion. FAMEs of ECO were investigated as being possibly suitable for
use as a promising biodiesel feedstock [26]. Castor oil is planted in
Upper Egypt and is widely distributed in the southern and south-
western regions with a total area of about 2,0 0 0,0 0 0 ha, and the
annual seeds production is above 250,700 tons [27]. The yield of
the seed castor oil is about 40–60%. In addition, the castor trees
are gaining importance due to its low maintenance and fewer crop
husbandry management practices required [27]. This paper aimed
to evaluate the biodiesel that is produced from alkali transesteri-
fication of Egyptian castor oil using ASTM standards, and to com-
pare its fuel properties with fossil-based fuel (petroleum diesel),
and compare different diesel-biodiesel blends with different ratios.
2. Materials and methods
2.1. Extraction of castor oil
Dry castor seeds (500 g) were crushed using a domestic grinder
and the oil was extracted by petroleum ether using a Soxhlet ap-
paratus at 45–50 °C for 6–8 h until the extraction was completed.
The oil content was determined as the difference in weight of the
dried castor seeds before and after the extraction (38%). The deter-
mination was performed in triplicate, and the amount of obtained
oil was considered as the average [28].
2.2. Treatment of extracted castor oil
The conversion of castor oil into biodiesel was performed by
two steps. The first is esterification of free acids in the oil by
methanol using H2 SO4 as a catalyst to decrease the amount of free
acids in the oil. The second is transesterification of the treated oil
by sodium methoxide [29].
2.3. Free fatty acid esterification
In a round flask (10 0 0 mL) equipped with Dean-Stark appara-
tus connected to a condenser, castor oil (513 g; 1.1 mol) was mixed
with methanol (192 g; 6 mol) and stirred. Sulfuric acid (7.6 ml; 0.76
wt% of oil) was added slowly and reaction mixture was refluxed.
After 1–1.5 h refluxing, the reaction was monitored by IR spec-
troscopy and TLC, showing esterification of free fatty acids present
in the castor oil [30].
2.4. Alkaline transesterification
In the transesterification reaction with refined castor oil, the
treated oil (1 mol) was charged into the reactor, followed by slow
addition of methanol (6 moles). The mixture was stirred with heat-
ing at 55 °C and Na–methoxide (1% of oil) was added as a cata-
lyst. After 2 h of refluxing, two phases were obtained, the upper
is the biodiesel phase and the lower is glycerine phase. The upper
biodiesel layer was separated and the excess methanol was filtered
off under reduced pressure and then washed by deionized water
to remove the traces of glycerin and catalyst [31].
2.5. FAME analysis
The FAME of castor oil was identified by gas chromatography-
mass spectrometry (GC–MS). The hexane (1 μL) extract was
Please cite this article as: N.A. Negm et al., Preparation and evaluation of biodiesel from Egyptian castor oil from semi-treated industrial
wastewater, Journal of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.02.024
[m5G;March 3, 2016;16:20]
injected into a highly polar HP Innowax capillary column with a
length of 30 m (inner diameter 0.32 m, film thickness 0.5 mm, split
1:20). An Agilent 6890 (CA, USA) equipped with a flame ioniza-
tion detector was used. The injector and detector temperatures
were 250 and 280 °C, respectively. The oven temperature was pro-
grammed from 190 °C holding at 3 min to 240 °C at the rate of
15 °C /min for 17 min. The carrier gas was high-purity hydrogen.
The peaks of FAME were identified by comparing their retention
time with that of the known standards, carried out under similar
separation conditions. Peak integration was performed by applying
HP3398A software. Each FAME determination was run in triplicate
and averages were reported.
2.6. Castor oil and biodiesel specifications
The following data were determined for castor oil: refraction
index, saponification value, iodine value, acid value, photometric
color, water content, and oil percent in castor seeds. The character-
istic specifications of the produced biodiesel including: kinematic
viscosity (at 40 °C and at 100 °C), iodine value, density, cetane
number, pour point, cloud point, ash %, carbon residue %, flash
point, and fire point were also determined. The mentioned proper-
ties were determined according to AOCS methods and ASTM spec-
ifications [32–40].
2.7. Engine test
The engine tests of the biodiesel and diesel-biodiesel blends
were performed using a direct injection four stroke single cylin-
der diesel engine of capacity 624 cm3 . The running speed of the
engine was 1500 rpm, and the tests were carried out at five differ-
ent loads of: 6.37, 12.74, 19.11, 22.3 and 25.48 N. Four fuels were
used in the tests: regular diesel fuel, and three blends of regu-
lar diesel with: 10% biodiesel (B10), 20% biodiesel (B20) and 40%
biodiesel (B40). The fuel volume used in each run was 50 cm3 and
the time of its consumption (sec) and the brake power (kW) were
recorded for each fuel type. The break specific fuel consumption,
BSFC (gm/kWh) and the break thermal efficiency, BTE (%) were cal-
culated according to the following formulations:
BSFC = (Fuel consumption rate )/(Brake power )
BTE = (Brake Power × 360 0 0 0 )/(Fuel consumption rate
× Calorific value )
where: fuel consumption rate in gm/h, brake power in kW, and
Calorific value in kJ/g.
3. Results and discussion
3.1. Fatty acid composition and properties
The fatty acid content (FAC) of the used castor oil is shown in
Table 1. The fatty acids in castor oil were determined as: palmitic
acid (C16:0), stearic acid (C18:0), oleic acid (C18:1), linoleic acid
(C18:2), linolenic acid (C18:3), and recinoleic acid (C18:1:OH). The
predominant fatty acids found were linoleic acid and recinoleic
acid. A total of six different fatty acids were identified in percent-
ages of the total fatty acid of the castor oil. In this study, recinoleic
acid had the highest percentage of total fatty acids (81.93%);
linoleic acid had the second highest percentage (6.33%). Ramos
et al. [41] suggested that the ideal vegetable oil composition for
biodiesel includes a high percentage of monounsaturated fatty
acids, in addition to low proportions of polyunsaturated acids and
a minimum content of saturated fatty acids. Based on these prin-
ciples, the castor oil under study is an ideal feedstock for biodiesel
production. The other properties identified for the used castor oil
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N.A. Negm et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–6 3

Table 1 3.2.1. Iodine value

Fatty acid composition and physical properties of castor oil.

Property Value The iodine value is an index that quantifies the degree of un-
saturation of biodiesel, and its high value is attributed to the ten-
Fatty acid composition: Percent:
Palmitic acid (C16:0) 2.17
dency to polymerization and formation of deposits on injection
Stearic acid (C18:0) 2.35 nozzles and on piston rings [42]. The iodine value of castor oil
Oleic acid (C18:1) 5.46 biodiesel (Table 2) is found to be (82.7 g I2 /100 g oil) compared
Linoleic acid (C18:2) 6.33 to sunflower oil biodiesel (108.2 g I2 /100 g oil), soybean (128 g
Linolenic acid (C18:3) 1.76
I2 /100 g oil) [43] and rapeseed (109 g I2 /100 g oil) [43] which in-
Recinoleic acid (C18:1:OH) 81.93
dicates that castor oil-based biodiesel is more stable compared
Photometric color 4.34
to other biodiesels above. The iodine value of castor oil based
Saponification value 198.6 mg/g oil
Iodine value 82.7 g I2 /100 g oil biodiesel is below the specification of EN 14214 [44] maximum
Acid value 3.3 mg KOH/gm limit (120 g I2 /100 g oil).
Refraction index 1.48
Water content 5% 3.2.2. Cetane number
yield 38%
The cetane number (CN) defines the ability of fuel to ignite
quickly after being injected. Higher value of (CN) indicates better
were: photometric color, saponification value, iodine value, acid ignition quality of fuel. This is one of the most important parame-
value, refraction index, and water content. The result obtained for ters, which is considered during the selection of methyl esters for
the percentage oil content was 38%. This relatively high yield may use as biodiesel. Biodiesel standards of the USA (ASTM D6751) [45],
be as a result of environmental factor which enhance the growth and European Organizations (EN 14214) [44] have set this value as
and productivity of the seed. This value falls within the range 47, and 51, respectively. The cetane number was 55.82 in case of
value of 30–55% reported by Aldrich [28]. This yield makes the the biodiesel obtained from the studied castor oil (Table 2). The
industrial practice of the oil recovery a profitable venture. higher value of cetane number of the produced biodiesel from cas-
The conversion of the oil to fatty acid methyl esters was tor oil represents its high ability towards ignition in engines after
followed by monitoring the area under peak at 1460 cm−1 and injection.
1436 cm−1 of IR spectroscopy of the formed FAME. The area under
peaks represents the amount of formed FAME during the trans- 3.2.3. Density
esterification reaction by using a standard FAME. It is clear from Density is an important parameter for airless D2 combustion
Fig. 1 that the area increased by increasing the time of reaction. systems. The density of methyl esters increases with the increas-
The transesterification reaction was further followed by using TLC ing number of double bonds [46]. Sunflower oil based biodiesel,
method. The spot separation identified the purity and the end having a lower amount of saturated esters (8.7%), showed a
point of the reaction, which confirmed the results obtained from higher density (0.900 g/cm3 ), while S. foetida biodiesel having a
IR spectroscopy, Fig. 2. high amount of saturated esters (32.3%) showed a lower den-
sity (0.850 g/cm3 ). The density of the obtained castor oil biodiesel
3.2. Biodiesel properties was (0.878 g/cm3 ), which is comparably lower than the densities
of soybean (0.885 g/cm3 ) [47], and high oleic rapeseed oil (0.88–
The determined fuel properties of the prepared biodiesel were: 0.888 g/cm3 ) based biodiesels [47]. The standard for biodiesel
iodine value, cetane number, density, viscosity (40 °C, 100 °C), flash states that the density should have 860–900 kg/m−3 in EN 14214
point, fire point, cloud point, pour point, ash and carbon residue %. [44] and 820–900 kg/m−3 in GB/T 20828 [46]. The result obtained

Fig. 1. IR spectroscopy follow-up of castor oil transesterification reaction using 1% sodium methoxide.

Please cite this article as: N.A. Negm et al., Preparation and evaluation of biodiesel from Egyptian castor oil from semi-treated industrial
wastewater, Journal of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.02.024
JID: JTICE
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Fig. 2. TLC profile of the transesterification product using 1% sodium methoxide.

Table 2 literature [52]. The kinematic viscosity of castor oil biodiesel at

Fuel properties of the biodiesel obtained from the studied
100 °C was 1.26 cSt, which is a low value compared to different
castor oil.
biodiesels obtained from Sunflower, Sterculia foetida, Camelina and
Biodiesel property Value Palm oils.
Iodine value 82.7 g I2 /100 g oil
Cetane number 55.82 3.2.5. Flash point
Density 0.878 g/cm3 The flash point is the temperature at which the fuel becomes
Kinematic viscosity @ 40 °C 4.65 cSt a mixture that will ignite when exposed to a spark or flame. Since
Kinematic viscosity @ 100 °C 1.28 cSt biodiesel has a higher flash point than diesels, it is a safer fuel than
Carbon residue % 0.052
diesel [53]. Biodiesel is considered safer to transport and handle
Ash % 0.025
Pour point, °C −15 because of its considerably higher flash point compared to Diesel
Cloud point, °C 0.0 No. 2. Typically, biodiesel with no or very minimal methanol carry
Flash point °C 151 over exhibits flash point within the range of 160 to 180 °C depend-
Fire point °C 156
ing on its FAME composition. While, flash point of diesel No. 2 only
is in the range of 58 to 62 °C [54]. However, biodiesel containing
only 0.2 and 0.3% methanol resulted in a significant lowering of
for castor oil biodiesel (Table 2) showed that the methyl ester of the flash point to as low as 106 and 78 °C, respectively (Table 2).
transesterified castor oil was within the specification limits of two The flash point of biodiesel is also affected by its FAME compo-
standard deviations (Table 2). The density value of castor oil based sition, more importantly; the biodiesel flash point is reported to
biodiesel was found to be in the range of EN specifications (0.86– assess the possible methanol carry over in the final product. Cas-
0.90 g/cm3 ) [45]. tor oil biodiesel showed a slightly lower flash point (151 °C) com-
pared to the sunflower (177 °C), soybean (171 °C) [43] and rapeseed
3.2.4. Kinematic viscosity (170 °C) [43] biodiesels. It is evident that flash point of castor oil
Kinematic viscosity represents flow characteristics and the ten- biodiesel is well within the specifications of ASTM (>130 °C) and
dency of fluids to deform with stress. Kinematic viscosity is a EN (>101 °C) standards.
more important parameter than density regarding fuel atomiza-
tion as well as fuel distribution [48]. Kinematic viscosity is ex- 3.2.6. Cloud point
pressed in centistokes (cSt) (Table 2). It is well accepted that a The cloud point is defined as the temperature at which a cloud
biodiesel comprised mainly of longer chain FAME exhibits higher of wax crystals first appears in a liquid when it is cooled. In gen-
kinematic viscosity [49,50]. On the other hand, the presence of eral, wax crystals occur in two phases: nucleation and growth of
unsaturated components resulted in biodiesel with lower viscos- crystals. The cloud point of biodiesel occurs during the start of
ity. Knothe and Steidley [49] also demonstrated that with the wax cluster formation involving higher molecular weight compo-
same chain length, the additional double bond in a polyunsatu- nents to give visible crystals [55–57]. By continuous cooling of the
rated FAME (e.g. linoleate vs oleate) does not result in a signif- sample, the agglomeration occurs. At this point, it involves the in-
icant reduction in viscosity as does the first double bond (e.g. teraction between the high and low melting components to give
oleate vs stearate). For biodiesel, the kinematic viscosity at 40 °C bigger crystals. Cloud point measurement is a standard test which
should be between 1.9 and 6.0 cSt [51] in ASTM, and 3.5–5.0 in applied to measure the flow properties of biodiesel during oper-
EN specifications. The obtained kinematic viscosity value of the ating in cold weathers [56]. The cloud point depends upon the
castor oil biodiesel was within the range of ASTM and EN speci- feedstock used and must be taken into consideration if the fuel is
fications. The kinematic viscosity (at 40 °C) of castor oil biodiesel to be used in cold environments [58]. The cloud point of the cas-
is slightly higher (4.65 cSt) compared to those published for sun- tor oil biodiesel is found to be 0 °C which is lower in value when
flower oil (4.52 cSt), soybean (4.2 cSt) [43] and rapeseed (4.4 cSt) compared to sunflower oil biodiesel (1 °C), and higher than the
[43] biodiesels. The values obtained in this study for castor oil biodiesels obtained from soybean oil (−2 °C) [59] and rapeseed oil
biodiesel viscosity was comparable to the values reported in the (−4 °C) [59]. Nevertheless, cloud point value of the biodiesel from

Please cite this article as: N.A. Negm et al., Preparation and evaluation of biodiesel from Egyptian castor oil from semi-treated industrial
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Table 3
Engine test results for regular diesel and diesel-biodiesel blends.

Fuel Load, Brake power, Load, Fuel volume Time of fuel consumption, Fuel consumption, BSFC, Brake thermal efficiency,
N kW (N.m) (mL) (sec) g/hr gm/kWh %

Regular diesel 6.37 1 6.37 50 232.3 651 651 15

12.74 2 12.74 50 208 727 363.5 24.2
19.11 3 19.11 50 177.8 850.4 283.4 28.26
22.3 3.5 22.3 50 155.92 964.7 275.6 29
25.48 4 25.48 50 121 1249.5 312.37 25
B10 6.37 1 6.37 50 263.46 573.9 573.9 14.11
12.74 2 12.74 50 201.13 751.75 375.8 21.5
19.11 3 19.11 50 158.93 951.36 317.12 25.5
22.3 3.5 22.3 50 136.3 1109.3 316 25.63
25.48 4 25.48 50 127.5 1185.9 296.4 27.63
B20 6.37 1 6.37 50 260.57 580.26 580.26 14.12
12.74 2 12.74 50 181.11 834.85 417.6 19.64
19.11 3 19.11 50 159.73 946.6 284 28.8
22.3 3.5 22.3 50 140.05 1079.6 308.28 26.6
25.48 4 25.48 50 118.61 1274.76 318.69 25.7
B40 6.37 1 6.37 50 178.75 846 846 9.7
12.74 2 12.74 50 160.92 940 470 17.44
19.11 3 19.11 50 145.22 1040.6 347 26.19
22.3 3.5 22.3 50 116.1 1302.3 378 21.7
25.48 4 25.48 50 101.5 1490 372.5 22

castor oil is within the range of ASTM specifications (−3 to 12 °C)
(Table 2).
In addition to the above studied parameters, the carbon and
ash percentages in the biodiesel of castor oil were 0.052% and
0.025%, which are very low values and did not cause any potential
on the environment when ignited. The pour point of the obtained
biodiesel was in the range of the standard values (0 °C). Further-
more, the concentration of linolenic acid and acids containing four
double bonds in FAME should not exceed the limit of 12% and 1%,
respectively, in accordance with European standard organizations
[60]. The linolenic acid of the castor oil was (1.76%) which is much
lower than 12%, while it did not contain fatty acids with four dou-
ble bonds.
3.3. Engine performance of castor oil biodiesel
The results of engine testing using: regular diesel fuel (D),
blend of regular diesel fuel with 10% castor oil biodiesel (B10),
blend of regular diesel fuel with 20% castor oil biodiesel (B20),
and a blend of regular diesel fuel with 40% castor oil biodiesel
(B40) are listed in Table 3. It is clear that the performance of the
diesel engine at full loading has been improved by blending regu-
lar diesel fuel with 10% biodiesel whereby the brake specific fuel
consumption has been decreased from 312.37 gm/kWh using solar
to 296.4 gm/kWh using B10 blend. The estimated brake thermal ef-
ficiency has been also increased due to blending with 10% biodiesel
from 25% to 27.36%. However, the reverse was true if the percent-
age of biodiesel has increased over 10%. The brake specific fuel
consumption was 372.5 gm/kWh using 40% blend of biodiesel com-
pared to 312.37 gm/kWh using regular diesel (Table 3). The thermal
efficiency was also lower using such bend being 22% compared to
25% using regular diesel.
4. Conclusions
The fuel properties of biodiesel obtained from alkaline trans-
esterification of castor oil were determined using standard meth-
ods and compared with literature reported methyl esters of several
biodiesel oils obtained from sunflower oil, soybean and rapeseed
oils. The results of biodiesel were in acceptable range compared to
the standard values of European and ASTM specifications. Further-
more, the thermal and engine properties of the castor oil biodiesel
were comparable to regular diesel.
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