Biofuels

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Comparative analyses of biodiesel produced

from jatropha and neem seed oil using a gas
chromatography–mass spectroscopy technique

M.U. Kaisan, S. Abubakar, B. Ashok, Dhinesh Balasubramanian, S. Narayan,

Ivan Grujic & Nadica Stojanovic

To cite this article: M.U. Kaisan, S. Abubakar, B. Ashok, Dhinesh Balasubramanian, S. Narayan,
Ivan Grujic & Nadica Stojanovic (2018): Comparative analyses of biodiesel produced from jatropha
and neem seed oil using a gas chromatography–mass spectroscopy technique, Biofuels, DOI:
10.1080/17597269.2018.1537206

To link to this article: https://doi.org/10.1080/17597269.2018.1537206

Published online: 24 Dec 2018.

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BIOFUELS
https://doi.org/10.1080/17597269.2018.1537206

Comparative analyses of biodiesel produced from jatropha and neem seed oil
using a gas chromatography–mass spectroscopy technique
M.U. Kaisana , S. Abubakara , B. Ashokb, Dhinesh Balasubramanianc, S. Narayand , Ivan Grujice and
Nadica Stojanovice
a
Ahmadu Bello University, Nigeria; bVIT University, India; cMepco Schlenk Engineering College, India; dMechanical Engineering
Department, Qassim University, Saudi Arabia; eFaculty of Engineering, University of Kragujevac

ABSTRACT ARTICLE HISTORY

Biodiesel from jatropha, neem and cottonseed were produced and their compositions were ana- Received 5 April 2018
lyzed using gas chromatography–mass spectroscopy. The results revealed that the jatropha, neem Accepted 21 August 2018
and cottonseed oils are reliable sources of biodiesel and are renewable, and hence have a poten-
KEYWORDS
tial to partially meet energy demands in an eco-friendly manner. The biodiesels produced from
Biodiesel; jatropha; neem;
jatropha contained 91.97% methyl ester, and that produced from neem contained 70.2% methyl gas chromatography; mass
ester, whereas that produced from cotton contained 89.75% methyl ester.The greater proportion spectroscopy
of prolific ester in the jatropha biodiesel is mono-saturated methyl octa-decanoate which
contributes 53.44% by volume. This ester has the tendency of assigning stability to biodiesel. For
neem-based biodiesel, the profile evaluation revealed that octadecanoic acid methyl ester is the
dominant compound in the mixture with 54.69% by volume. For cotton, the profile revealed that
the methyl octadecenoate (C19H36O2) is the predominant compound in the mixture, having the
highest percentage of 17.72%. The physico-chemical analyses of the three biodiesels has indicated
that the three conform with the American Society for Testing and Materials (ASTM) standards for
specific gravity, viscosity, acid value, cold flow properties and sulfur content, and hence are
suitable for use in compression ignition engines. Statistical analyses confirmed that there was no
significant difference between the experimental values of all the physico-chemical properties inves-
tigated; therefore, the experimental data is validated.

Introduction seed oil with high free fatty acids (15%FFA). The high FFA
level was esterified to less than 1% by a two-step pretreat-
Biodiesel is the most promising source of renewable energy
ment process. The first step was carried out with a 0.60 w/
with high potential to replace petroleum-based diesel fuel,
w methanol-to-oil ratio in the presence of 1% w/w H2SO4
owing to similarities in physico-chemical properties
as an acid catalyst in 1 h reaction time at 50
C. After the
between diesel fuels and the biodiesel (Ghorbani et al.
reaction, the mixture was left to settle for 2 h and the
2011). Biodiesel can be defined as simple alkyl esters of methanol–water mixture separated at the top layer was
fatty acids produced from vegetable oils and animal fats. removed. The second step was transesterified using 0.24
Several plants found in Nigeria have good capacity to pro- w/w methanol:oil and 1.4% w/w NaOH to oil as alkaline
duce biodiesel-based fuels (Nafiu et al. 2011). According to catalyst to produce biodiesel at 65
C. The final yield for
Nigeria National Petroleum Corporation (NNPC)-approved methyl esters of fatty acids, ca. 90%, was achieved in 2 h.
ethanol policy, biodiesel represents fatty acid methyl esters Furthermore, He et al. (2009) investigated the effect of
(FAMEs) or mono-alkyl esters originating from vegetable oil browning on callus morphology and biochemical indices.
or animal fats. The quality specifications are predetermined Light microscopy and scanning electron microscopy showed
by the Standards Organization of Nigeria (SON), striking differences in callus morphology. Gas chromatogra-
Department of Petroleum Resources (DPR) and any other phy–mass spectrometry (GC-MS) results showed that satu-
relevant governmental institutes (Kaisan, 2013). One major rated and unsaturated fatty acid quantities differed
aim of these organizations is to develop biodiesel-based significantly but there was little difference in fatty acid com-
fuels (Haresh, 2008). In the United States, to a large degree, position between non-browning and browning callus.
the focus of biodiesel is on soybean-based oil (EIA, 2013). Moreover, Martı et al. (2010) conducted a preliminary
In another development, Woo et al. (2016) worked on investigation on the suitability of numerous non-edible oil
the direct (trans)esterification of whole Jatropha curcas L. seeds for production of bio- diesel and other yields. The oil
kernels in subcritical solvent mixture of water, methanol seeds represented were jatropha (Jatropha curcas), neem
and acetic acid. A high FAME yield of 96.56% was attained (Azadirachta indica), moringa (Moringa oleifera), trisperma
at a solvent (water:acetic acid:methanol 1.25:5:15, v/v/v)-to- (Aleurites trisperma), castor beans (Ricinus communis) and
solid ratio of 7 cm3/g. candlenut (Aleurites moluccana). The highest oil content
Similarly, Johanes and Hirata (2008) worked on a (62.0% w/w) was found in trisperma seeds, but the use of
method of biodiesel production from crude Jatropha curcas that oil for biodiesel production is restricted by its high

CONTACT S. Narayan [email protected] Qassim university Saudi Arabia

ß 2018 Informa UK Limited, trading as Taylor & Francis Group
2 M. KAISAN ET AL.

content of polyunsaturated fatty acids. The oils of castor species can be feasible, cost effective and environmen-
beans and moringa contained 86.0% ricinoleic acid and tally friendly.
70.6% oleic acid, respectively, while in the oils from the Tariq et al. (2011) synthesized biodiesel from rocket
other seeds no predominance of any acid was observed. seed oil by base-catalyzed transesterification with metha-
According to the oil yield and to the fatty acid composition nol. The synthesis of biodiesel was confirmed by FT-IR and
of the oil, jatropha was acknowledged as the most auspi- Nuclear Magnetic Resonance (NMR) (1H and 13C) spectros-
cious oil seed for biodiesel production. copy. Various fuel properties of the synthesized biodiesel
Also, Pramanik (2003) investigated the high viscosity of were determined using ASTM methods and discussed
jatropha oil which has been deliberated as a potential sub- accordingly. A total of 11 FAMEs were identified in rocket
stitute fuel for compression ignition (CI) engines; the vis- seed oil biodiesel by the retention time and the fragmenta-
cosity was decreased by blending the biodiesel with diesel. tion pattern data of GC-MS analysis. The identified FAMEs
The blends of variable proportions of jatropha oil and die- were methyl 9-hexadecenoate (C16:1), 14-methyl pentade-
sel were set, investigated and matched with diesel fuel. canoate (C16:0), methyl 9,12-octadecadienoate (C18:2),
The performance of the engine using blends and jatropha methyl 9-octadecenoate (C18:1), methyl octadecanoate
oil was evaluated in a single-cylinder CI engine and com- (C18:0), methyl 11-eicosenoate (C20:1), methyl eicosanoate
pared with the performance obtained with diesel. (C20:0), methyl 13-docosenoate (C22:1), methyl docosa-
Significant improvement in engine performance was noate (C22:0), methyl 15-tetracosenoate (24:1) and methyl
observed compared to vegetable oil alone. From the prop- tetracosanoate (C24:0). The percentage conversion of trigly-
erties and engine test outcomes it has been proven that cerides to corresponding methyl esters determined by 1H
jatropha oil can replace 40–50% diesel without any NMR was 88.49%.
engine alteration. Zhou et al. (2006) established that biodiesel is manufac-
In another development, Rodrı et al. (2011) evaluated tured by transesterification of animal fat or vegetable oil. The
some properties of the oils and derivative fatty acid ethyl reactants (oil and methanol) and the products (FAME and gly-
esters from two different types of jatropha planted in cerol) are partially mutually soluble in the reaction process.
Cuba. The properties they investigated included the acid Intersolubility of the reaction components is essential data for
value, peroxide value, p-anisidine value and fatty acid ethyl production design and process operation. In this work, the
ester composition. The two farms were in San Jose (SJ) and jatropha oil was transesterified to give jatropha oil FAME.
Guantanamo (Gt), corresponding to the western and east-
ern part of the island. The study shows that the jatropha Advantages of biodiesel
acquired from Guantanamo has a higher acid value and
peroxide value compared with that from San Jose. The p- Biodiesel-based fuels have many advantages over petrol-
anisidine values did not show a clear trend and the results eum diesel as readily established in the existing literature.
of GC-MS indicated a similar composition. The results Some of these advantages include biodegradability, liquid
obtained by GC are in good agreement with previ- nature, portability, low toxicity, availability, lower NOx emis-
ous reports. sions, environmental friendliness, better lubricating proper-
Sardar et al. (2011) worked on the biodiesel production ties and higher flash point (safer to handle and store), ease
and characterization of FAMEs synthesized from a novel of blending with diesel, extended life span of CI engines,
source, non-edible neem oil. FAMEs were produced job creation, providing green cover to waste land and
through methlanolysis of neem oil using methanol in the reduction of dependency on imported refined oil. In add-
presence of NaOH and KOH as catalysts. Conversion of ition, higher cetane number improves ignition and combus-
crude neem oil to biodiesel was 76.8%. Fuel properties of tion quality (Akande and Olorunfemi, 2009; Belewu, 2011;
neem oil biodiesel (100%), i.e. flash point (124
C), viscosity Madarasz and Kumar, 2011; Izah and Ohimain 2012;
(4.91 at 40
C), density (0.8785 at 15
C kg/L), and color Simonyan and Fasina, 2013; Bugaje, 2014).
(2.5), were close to American Society for Testing and
Materials (ASTM) biodiesel standards. Fuel properties of
Disadvantages of biodiesel
biodiesel blends were also in accordance with ASTM stand-
ards. Quality and quantity of neem oil biodiesel, based on The disadvantages of biodiesel include higher production
physico-chemical characteristics, were determined using cost, reduced cold flow properties, detergent characteristics
analytical techniques, such as GC-MS, nuclear magnetic res- in fuel tanks, higher viscosity, lower volatility and reactivity,
onance, and Fourier transform infrared (FT-IR) analysis. It is higher fire point (producing carbon deposits) and corro-
concluded that the rise in the use of non-edible oil bio- siveness (Ghorbani et al. 2011; Izah and Ohimain 2012).
diesel is inevitable and neem is the potential source in this The following challenges have been identified with bio-
scenario of a promising source of renewable energy. diesel in the established literature: competition with food
Gangadhara and Prasad (2016) worked on the optimiza- security and pharmaceutical demands for the feedstock,
tion of the transesterification process and analysis of bio- feedstock supply shortage, poor quality of feedstock, proc-
diesel from non-edible oilseeds of neem and Pongamia essing challenges, technological challenges and poor policy
converted into FAMEs through base-catalyzed transesterifi- framework (Izah and Ohimain, 2012; Kaisan et al. 2015).
cation using an optimum ratio of 1:6 oil: methanol at 60
C.
Biodiesel from these sources was analyzed for qualitative
Feedstocks used for biodiesel production
and quantitative characterization using GC-MS and FT-IR
techniques. Based on qualitative and quantitative analysis The potential economic and social benefits of modern bio-
of biodiesel, it is concluded that the biodiesel from these mass energy arise from the fact that agriculture could face
 BIOFUELS 3

enormous demand for the feedstock. The feedstock will been investigated by Ohimian (Izah and Ohimain
need to be produced, harvested, transported, converted 2012). Mansourpoor and Shariati (2012) Worked on
into biodiesel, blended, stored and distributed for final util- optimization of biodiesel production from sunflower
ization (Akande and Olorunfemi, 2009). In India, only about oil using response surface methodology. Moser
12 of almost 100 varieties of feedstocks have been tapped (2009) Reviewed properties of various feedstocks.
so far, with focus on mahua-, jatropha-, neem- and karanja-  Topare et al. (2011) produced biodiesel from microal-
based biodiesel (Madarasz and Kumar, 2011). gae. Chalatlon et al. (2011) produced biodiesel from
Feedstocks used for biodiesel include soybean oil, palm jatropha oil and investigated its use in direct-injec-
oil, castor oil, Parkia biglobossa, jatropha, sunflower oil, tion diesel engines (Kaisan et al. 2015).
coconut oil, rapeseed oil, groundnut oil, neem seed oil,  Other methods of biodiesel production, for instance
peanut oil, cottonseed oil, tobacco, dessert date, castan- using superficial methanol technology, have been
hola, rubber tree, tung, Abyssinian mustard, false flax or recorded (Saka et al. 2006).
gold of pleasure, polanga, cardoon, sesame, marula, pump-
kin, jajoba (Madarasz and Kumar 2011; Izah and Ohimain The aim of this research is to produce biodiesel from
2012; Kannahi and Arulmozhi, 2013; Kaisan et al. 2016). The jatropha, neem and cotton and to determine their percent-
majority of these seeds are found in Nigeria. age composition using GC-MS analyses, as well as to com-
Non-edible biodiesel feedstocks include almond oil, kar- pare the quantity and quality of the various biodiesels
anja oil, castor bean, hemp, jatropha, ratanjot, Pongamia produced. Production of biodiesel was done using the
pinnata, Callophylum inophyllum or nagchampa, Hevea bra- alkali transesterification method. Despite all the valuable
silinsis or rubber seed, Calotropis gigantia or ark, Euphorbia research that has been carried out in the area of study, a
tirucalli or sher, Boswellia ovalifoliotata, neem seed and gap has been left in the area of comparing the biodiesel
Madhuca indica (Madarasz and Kumar, 2011; Kannahi and products of different promising feedstocks such as jatro-
Arulmozhi, 2013). Other biodiesel feedstocks include myco- pha, neem and cotton. Hence, this research addresses
biodiesel, fungal biodiesel and Aspergillus niger (Kannahi this gap.
and Arulmozhi, 2013, Adejuwon and Olorunfemi, 2010).
Methodology
Biodiesel blending Sample preparation
Blending simply means mixing of biodiesel with petroleum- Biodiesel production
based diesel. Biodiesel with nomenclature B5 means 5% Various samples from neem seeds and jatropha seeds were
biodiesel blended with 95% diesel. Similarly, B10 refers to a procured and biodiesel was produced from each sample
mixture of 10% biodiesel with 90% diesel. There are higher using the alkali transesterification reaction method. A given
ratios such as B15, B20, B30, B50, etc. B100 refers to a pure mass (0.40g) of sodium hydroxide (NaOH) was added to
biodiesel. Nigeria is committed to blending biodiesel up to 40 cm3 of methanol and stirred until it was com-
20% by volume (Izah and Ohimain, 2012). pletely dissolved.
According to Stark et al. (2010), blending biodiesel with One hundred grams of jatropha oil was placed in a flask
hydrocarbon blend stock can be done in any of the follow- and the methanol-based sodium hydroxide solution was
ing ways: added to it. The mixture was stirred for 20 min at 25
C and
then poured into a separating funnel (Kaisan et al. 2013).
 In-line blending: Here two tanks are involved, one The process was repeated for neem and cotton oilseeds.
containing biodiesel and the other having refined
petro-diesel. Both of these are passed through a pipe
and hose and are mixed in a particular ratio before Blending
being collected in a third tank. A temperature of The blending was done for each biodiesel type with petrol-
60
C above cloud point is required to avoid the risk eum diesel alone. Each biodiesel sample was blended with
of shock crystallization (Stark et al. 2010). fossil diesel in a ratio of 5:95, 10:90, 15:85, 20:80, 25:75 and
 Splash blending: This is done by pumping biodiesel 30:70 by volume and a pure sample of each biodiesel as
at a temperature range of 180–200
C into a tank well as a pure diesel sample were kept for control pur-
containing diesel at about 80
C. This method is asso- poses. The blends were denoted B5, B10, B15, B20, B25,
ciated with quality rejection risk and as such is rarely B30 and B100 for the biodiesel blends (with J for jatropha
practiced (Stark et al. 2010). and N for neem) and B0 for the pure petroleum diesel
 Injection mixing: This is the blending of fuels in tanks (Kaisan et al. 2013).
at the manufacturing point before delivery to the
tankers. Control valves are used to ensure that a par-
GC-MS analyses
ticular quantity of biodiesel components is injected
alongside the petro-diesel (Stark et al. 2010). GC-MS analyses were carried out to determine the percent-
 There are substantive works on transesterification of age of methyl ester (biodiesel) present in B100J and
biodiesel from various feedstocks. The potential use B100N. The FAMEs composition of jatropha, neem and cot-
of waste cooking oil as an alternative feedstock for ton biodiesels was determined using GC-MS. Separation
biodiesel production has also been investigated was achieved via capillary column DB-5MS
(Chhetri et al. 2008; Caprita et al. 2005). Production (30 m  0.32 mm, 0.25 lm film thickness). The carrier gas
of biodiesel from oil palm feedstock in Nigeria has used was helium with a flow rate of 1.5 mL/min. The
4 M. KAISAN ET AL.

Table 1. Gas chromatography–mass spectroscopy results for jatropha biodiesel. Measurement of viscosity
Compound (methyl ester) Approximate composition (%) The viscosity was measured with a viscometer as shown in
Octadecanoic acid methyl ester C19H36O2 2.84 Figure 2 at a temperature of 313 K. According to Adebayo
Pentadecanoic acid methyl ester C17H34O2 14.25
Hexadecanoic acid methyl ester C16H32O2 2.67 et al. (2011) the viscosity at 40
C (313 K) is measured fol-
Octadecanoic acid methyl ester C19H36O2 19.32 lowing the ASTM D445 method using a calibrated viscom-
Octadecanoic acid methyl ester C19H36O2 15.10 eter with a calibration constant of 0.1057. In this research,
Octadecanoic acid methyl ester C19H38O2 9.62
Hexadecanoic acid methyl ester C16H30O2 15.10 determination of viscosity was done following the Institute
Octadecanoic acid methyl ester C18H36O2 2.51 of Petroleum (IP) method. This involves measuring the time
Eicosanoic acid methyl ester C21H42O2 3.11
Hexanoic acid methyl ester C19H38O4 1.35 of flow of the sample between two marked points on the
Docosanoic acid methyl esterC23H46O2 1.05 Ostwald viscometer (Nafi’u et al. 2012).
Octadecanoic acid methyl ester C21H40O4 5.05
Total 91.97 tt0
gsp ¼ (1)
t0
where:
Table 2. Gas chromatography–mass spectroscopy results for neem biodiesel.
Compound (methyl ester) Approximate composition (%) gsp ¼ specific vis cos ity
Pentadecanoic acid methyl ester C17H34O2 10.64
Hexadecanioc acid methyl ester C16H32O2 1.75
Octadecanoic acid methyl ester C19H34O2 9.52 t0 ¼ efflux time of solvent
Octadecanoic acid methyl ester C19H36O2 24.86
Octadecanoic acid methyl ester C19H38O2 9.97 t ¼ efflux time of solution
Octadecanoic acid methyl ester C18H42O2 10.34
Eicosanoic acid methyl ester C21H42O2 0.99 Flash point
Hexadecanioc acid methyl ester C19H38O4 2.13
Total 70.2 The flash point was determined by the ASTM D93 method
using a Pensky–Martens closed cup tester. The determin-
ation of the flash point of biodiesel was done in a tempera-
column temperature was programmed to heat from 120
C ture range of 60 to 190
C with the automated
to 300
C at a rate of 10
C/min as established by Tariq Pensky–Martens closed cup apparatus according to the
et al. (2011). The temperature of both injector and detector standard method of testing flash point. The flash point
was set at 200
C. A sample volume of 0.1 lL of each determination was carried out by heating a sample of the
methyl ester was injected using a rip mode, with a split fuel in a stirred container and passing a flame over the sur-
ratio of 1:10. The mass spectrometer was set to scan in the face of the liquid. If the temperature is at or above the
range of m/z 50–550 with electron impact (EI) mode of ion- flash point the vapour will ignite and an easily detectable
ization (Tariq et al. 2011). GC-MS analysis was used to study flash can be observed. The fire point will produce sufficient
the chemical composition of the synthesized biodiesel. vapour to maintain a continuous flame (Nafiu et al. 2011).
Major peaks were observed in the total ion chromatogram.
Each peak corresponds to a FAME content in each of the
biodiesels and was identified from the library match soft- Cetane number
ware (NO. NIST, 02). The identified FAMEs were verified by The cetane number was determined using a portable
running the standards under identical experimental condi- cetane/octane meter. The cetane index of the biodiesel–-
tions and comparing the respective retention time data diesel blend was determined by the ASTM D.976 method
which were confirmed by MS analysis. The results are as done by Kywe and Oo (2009).
shown in Tables 1 and 2 for jatropha and neem biodiesel,
respectively. Conditions adopted for the analyses are as fol- Cloud point. The cloud point was determined by visually
lows: column oven temperature of 60
C; injection tempera- inspecting for a haze to become visible as the fuel is
ture of 200
C; injection pressure of 112.8 kPa (Bosch-Fuste cooled in a cloud point and pour point tester, as shown in
et al. 2007; Yuan et al. 2008). Figure 3. This is the generally accepted method of testing
cloud point as reported by Kywe and Oo (2009).

Determination of physico-chemical properties

Pour point
The physico-chemical properties of the biodiesels were
The pour point was determined by the ASTM D.97 method
determined. These include parameters such as specific
(Kywe and Oo 2009). A 3.00 g sample of oil or biodiesel
gravity, flash point, calorific value, cetane number, copper
was placed into a test tube in which a thermometer was
strip corrosion, viscosity, total sulfur, aniline value, cloud
inserted through a cork which was used to cover the
point, pour point and acid value for all the samples.
mouth of the test tube. The test tube was then placed in
the cloud and pour point tester shown in Figure 4 and
Measurement of specific gravity observed at 10-min intervals for a period of 2 h. The test
The specific gravity of the samples was measured at room tube was removed and tilted to ascertain whether the oil
temperature using a Fisher brand hydrometer (size would flow or move, until it showed no movement when
0.795–0.910, accuracy 0.001) as shown in Figure 1. The the test tube was held horizontally for seconds (i.e. it had
measurement was performed according to a method solidified). The pour point was then taken at a temperature
adopted from Coronado et al. (2009). 5
C above the solid point.
 BIOFUELS 5

Figure 1. Fisher brand hydrometer.

Figure 2. Viscosity bath.

Figure 3. Cloud point and pour points tester.

6 M. KAISAN ET AL.

Figure 4. X-ray fluorescence (MWDXRF) spectrometer.

Calorific value (C23H46O2), at 3.11% and1.05% by volume. The profile

The calorific value of the biodiesel/diesel samples was revealed that octadecanoic acid methyl ester (C19H36O2) is
measured using a bomb calorimeter. A known amount of the dominant compound in the mixture, at 53.44% by vol-
fuel was placed in the crucible. The crucible was then ume. The FAME profile is the main factor that decides the
placed over a ring and a fine magnesium wire touching aptness or usefulness of any feedstock for production of
the fuel sample was stretched across the electrodes. The biodiesel fuel (Sokoto et al. 2011). The results in Figure 6
lid was tightly screwed and the bomb was filled with oxy- indicate that the most common ester in the jatropha-based
gen up to 25 atmospheres pressure. The initial temperature biodiesel is mono-saturated methyl octadecanoate. It is a
was recorded. The electrodes were then connected to a 6- very good compound that has the tendency to provide sta-
V battery and the circuit was switched on. The fuel in the bility to the biodiesel, because of the higher degree of
crucible burned with the evolution of heat. Heat liberated non-saturation in the fatty acid. Methyl esters limit its suit-
by burning of the fuel increased the temperature of the ability for use as a fuel due to a high polymerization ten-
water and the maximum temperature attained was dency which is caused by oxidation (Bamgboye and
recorded. The concepts of change in temperature and spe- Hansen, 2008; Sokoto et al. 2011).
cific heat were then used to compute the calorific values.
Neem oil methyl ester
Total sulfur content
The total sulfur content was determined using X-ray analy- The methyl ester content in the neem biodiesel as indi-
ses of the fuel samples as indicated in Figure 5. This test cated by the GC-MS analysis is depicted in Figure 7.
method covers the determination of total sulfur by mono- The main methyl esters are methyl octadecanoate
chromatic, wavelength-dispersive X-ray fluorescence (C19H36O2), methyl hexadecanoate (C17H34O2) and methyl
(MWDXRF) spectrometry in single-phase biodiesel and die- pentadecanoate (C16H32O2). Their respective percentages
sel fuels. The precision of this test method was determined are 54.69%, 3.88% and 10.64%. Another ester found in the
by an inter-laboratory study using representative samples biodiesel is eicosonoic acid methyl ester (C21H42O2) 0.99%.
of the fuels (Kaisan et al. 2013). The profile revealed that octadecanoic acid methyl ester
(C19H36O2) is the dominant compound in the mixture,
GC-MS results at 54.69%.
The FAME is the main factor that decides the aptness or
The results for methyl ester percentage contents of the otherwise of any feedstock for use in biodiesel fuel produc-
biodiesel products were analyzed by GC-MS of the tion (Sokoto et al. 2011). The results in Figure 7, just like
biodiesel produced from jatropha, neem and cotton oil the previous result, show that the most abundant ester in
seeds and are presented in Figures 6, 7, respectively. the neem diesel is monounsaturated methyl octadeca-
Interpretation of the peaks of the chromatogram is given noate. This is a very good compound that has the ten-
for each figure, paying more attention to the methyl esters dency to provide stability to the biodiesel, because the
present in each chromatogram only. higher degree of unsaturation in the FAMEs limits its suit-
ability for use as a fuel due to the high polymerisation ten-
Jatropha oil methyl ester
dency caused by peroxidation (Bamgboye and Hansen,
The methyl ester contents in the jatropha biodiesel as 2008; Sokoto et al. 2011).
portrayed by the GC-MS analyses are depicted by Figure 6. From Figures 5–7 and details of the results obtained
The main methyl esters are: methyl octa-decanoate from GC-MS, the percentage of methyl esters present in
(C19H36O2), methyl hexadecanoate (C17H34O2) and methyl the compounds of neem and jatropha is 70.2% and 91.97%
penta-decanoate (C16H30O2). Their respective percentages respectively. The GC-MS analyses confirmed that most of
by volume are 53.44%, 17.77% and 14.25%. the products are methyl ester compounds.
Other esters found in the biodiesel are eicosonoic acid At high temperatures, peroxidation can be accelerated
methyl ester (C21H42O2) and docosanoic acid methyl ester and an engine can quickly become gummed with
 BIOFUELS 7

Figure 5. Gas chromatography–mass spectroscopy chromatogram of jatropha seed biodiesel.

Figure 6. Gas chromatography–mass spectroscopy chromatogram of neem seed biodiesel.

polymerized fatty methyl esters; this is commonly experi- have been reported to be good feedstocks for biodiesel pro-
enced in CI engines (Gopinath et al. 2010). Hence, feedstocks duction (Carraretto et al. 2004). Their dominant esters are
with a high percentage of poly-unsaturated acid are not methyl octadecanoate and methyl hexadecanoate, similar to
suitable for usage as biodiesel. Since the dominant FAMEs those present in the cotton, jatropha and neem biodiesel.
for cotton, jatropha and neem biodiesel are methyl octade- Similarly, methyl octadecanoate and methyl hexadecanoate
canoate, methyl hexadecanoate and methyl pentadecanoate, were the dominant esters in rapeseed methyl esters with
which are monounsaturated, they might not have much percentage composition of 77.9 and 3.86%, respectively
affinity for oxygen that will lead to quick peroxidation. (Carraretto et al. 2004). Similar results were obtained for
These dominant esters are similar to the percentage of these Rhus succelanea L. and Annona reticulata as reported by
dominant esters are similar to the major FAMEs in Jatropha Demirabas (2005) and Demirabas (2008) respectively; hence,
curcas, consistent with the findings of Carraretto et al. it can be inferred that jatropha and neem biodiesels are sus-
(2004) whose results gave 51.7% and 14.3%, respectively tainable, renewable, reliable, combustible and suitable for
(Carraretto et al. 2004). Palm and olive oil methyl esters use in CI engines.
8 M. KAISAN ET AL.

Figure 7. Gas chromatography–mass spectroscopy results for cottonseed biodiesel.

Table 3. Methyl fatty acid esters of cottonseed biodiesel. Table 5. Viscosity of biodiesels and blends.
Compound (methyl ester) Approximate composition (%) Viscosity at 40
C (mm2/s)
Nonanoic acid methyl ester C10H18O3 0.20 B5 B10 B15 B20 B25 B30 B100
Octadecanoic acid methyl ester C19H36O2 3.49
Pentanoic acid methyl ester C17H34O2 11.53 Jatropha 4.92 4.37 5.22 5.60 5.56 5.88 6.00
Hexadecanoic acid methyl ester C18H36O2 0.54 Neem 4.19 4.52 5.20 5.61 6.20 6.76 6.00
Octadecadienoic acid methyl ester C19H34O2 14.23 Cotton 4.14 4.62 5.03 5.08 6.00 6.30 6.50
Octadecadienoic acid methyl ester C19H36O2 17.72 ASTM min 1.90 1.90 1.90 1.90 1.90 1.90 1.90
Octadecadienoic acid methyl ester C19H38O2 7.32 ASTM max 6.00 6.00 6.00 6.00 6.00 6.00 6.00
Oleic acid methyl ester C18H3O2 3.41 ASTM: American society of testing of material.
Eicosadienoic acid methyl ester C21H38O2 1.81
Octadecanoic acid methyl ester C19H38O2 1.49
Methyl ricinolate methyl ester C19H36O3 1.85
Eicosanoic acid methyl ester C21H42O2 3.47
feedstock for use in biodiesel fuel production (Sokoto et al.
Hexadecanoic acid methyl ester C19H38O4 7.07 2011). The results in Table 1 indicate that, the most abun-
Octadecenoic acid methyl ester C21H14O4 15.62 dant ester in the cotton diesel is monounsaturated methyl
Total 89.75
octadecanoate. It is a very good compound, it has the ten-
dency of assigning stability to the biodiesel, this is becau-
Table 4. Specific gravity of biodiesels and blends. se,higher degree of unsaturation in the FAMEs limits its
Specific gravity suitabilityfor use as a fuel (Bamgboye and Hansen, 2008;
B5 B10 B15 B20 B25 B30 B100 Sokoto et al. 2011). At high temperatures, commonly expe-
Jatropha 0.8704 0.8727 0.8763 0.8773 0.8783 0.8823 0.9072 rienced in combustion engines, peroxidation can be accel-
Neem 0.8734 0.8763 0.8783 0.8813 0.8843 0.8863 0.9497 erated and the engine can quickly become gummed with
Cotton 0.8714 0.8743 0.8763 0.8773 0.8793 0.8823 0.9145
Mixed 0.8720 0.8742 0.8757 0.8770 0.8849 0.8720 0.8712 polymerized FAMEs (Gopinath et al. 2010). Hence, feedstock
ASTM min 0.8000 0.8000 0.8000 0.8000 0.8000 0.8000 0.8000 with a high percentage of polyunsaturated acid is not suit-
ASTM max 0.9000 0.9000 0.9000 0.9000 0.9000 0.9000 0.9000
able for usage as biodiesel. Since the dominant FAMEs
ASTM: American society of testing of material.
methyl octadecanoate and methyl pentanoate are mono-
unsaturated they might have little affinity for oxygen which
will lead to rapid peroxidation. These dominant esters were
Cotton oil methyl ester
similar to the major FAMEs in J. curcus, having percentages
From Table 3, the main methyl esters present in the bio- of 51.7 and 14.3% respectively (Carraretto et al. 2004).
diesel are methyl nonanoate (C9H18O2), methyl hexadeca- Palm and olive oil methyl esters have been reported to
noate (C17H34O2) and methyl octadecenoate (C19H36O2). be good feedstocks for biodiesel production (Carraretto
Their respective percentages by composition were 0.20, et al. 2004). Their dominant esters are methyl octadeca-
0.54 and 17.72%. Other esters found in the biodiesel were noate and methyl hexadecanoate, similar to those present
methyl eicosanoate (C21H42O2), methyl pentanoate in the cotton biodiesel. Similarly, methyl octadecanoate
(C17H34O2) and methyl octadecenoate (C19H38O2), at and methyl hexadecanoate were the dominant esters in
respective percentages of 3.42, 11.5 and 1.49%. The profile rapeseed methyl esters with percentage composition of
revealed that the methyl octadecenoate (C19H36O2) was the 77.9 and 3.86% (Carraretto et al. 2004). This also conforms
predominant compound in the mixture having the highest to the results obtained for Rhus succelanea L. and Annona
percentage of 17.72%. The FAME profile is one of the key reticulata as reported by Demirabas (2005, 2008). Hence, it
factors that determine the suitability or otherwise of any can be inferred that cotton biodiesel is sustainable.
 BIOFUELS 9

Table 6. Calorific values of biodiesels and blends. Table 13. Analyses of variance for viscosity.
Calorific value Criteria Sum of squares df Mean square F Sig.
B5 B10 B15 B20 B25 B30 B100 Between groups 1.914 3 0.638 1.123 0.359
Within groups 13.635 24 0.568
Diesel 45.32 45.32 45.32 45.32 45.32 45.32 45.32 Total 15.549 27
Jatropha 42.84 43.72 42.99 44.21 45.41 42.1 44.23
Neem 43.09 42.16 43.11 44.66 42.98 43.02 43.13
Cotton 44.44 43.59 44.61 43.19 42.11 44.77 43.41
ASTM max 46 46 46 46 46 46 46 Table 14. Analyses of variance for acid values.
ASTM min 42 42 42 42 42 42 42 Criteria Sum of squares df Mean square F Sig.
ASTM: American society of testing of material. Between groups .201 3 0.067 38.739 0.000
Within groups .041 24 0.002
Total .242 27
Table 7. Acid values of biodiesels and blends.
Acid value (mg KOH/g)
Physico-chemical properties of biodiesels and blends
B5 B10 B15 B20 B25 B30 B100
from jatropha, neem and cotton compared with
Jatropha 0.31 0.34 0.40 0.36 0.42 0.44 0.48
Neem 0.16 0.14 0.18 0.12 0.20 0.20 0.24 ASTM standards
Cotton 0.24 0.28 0.22 0.18 0.18 0.20 0.18
ASTM max 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Results regarding the physico-chemical properties of jatro-
ASTM: American society of testing of material. pha, neem and cotton biodiesel along with their blends
are presented in Tables 4–11, for specific gravity, vis-
Table 8. Flash points of biodiesels and blends.
cosity, calorific value, flash point, acid number, pour point,
Flash point (
C)
and sulfur content.
The specific gravity of biodiesel from jatropha and neem
B5 B10 B15 B20 B25 B30 B100
and the ASTM standard values are given in Table 4. The
Jatropha 150 148 145 138 138 138 146
Neem 152 149 148 143 143 143 170
specific gravity values obtained in this study conform to
Cotton 167 150 150 145 145 145 155 the ASTM standard values. Hence, the quality of atomiza-
ASTM min 130 130 130 130 130 130 130 tion, combustion and fuel droplets as well as air–fuel mix-
ASTM max 170 170 170 170 170 170 170
Diesel 95 95 95 95 95 95 95
ing would be satisfactory while burning these binary and
ASTM: American society of testing of material.
multi-blends of cotton, jatropha and neem biodiesel.
The kinematic viscosity values of biodiesel from jatropha
and neem are given in Table 5. The viscosity values are
Table 9. Pour points of biodiesels and blends.
within the ASTM standards. The viscosity of a biodiesel
Pour point (
C)
influences the ease of starting an engine, the spray quality,
B5 B10 B15 B20 B25 B30 B100 the particle size, the quality of air–fuel mixing and the
Jatropha 9 9 12 6 15 15 3 penetration of the injected jet (Kaisan et al. 2017a;
Neem 9 9 6 6 6 9 6
Cotton 9 9 9 6 12 6 3
Enwerenmadu et al. 2014). Viscosity that is too low gives
ASTM min 15 15 15 15 15 15 15 low spray but leads to poor penetration, while a viscosity
ASTM max 10 10 10 10 10 10 10 that is too high causes operational problems at high
ASTM: American society of testing of material. temperature.
The calorific value is an important characteristic of fuels.
Table 10. Cetane number of biodiesels and blends. Table 6 gives the calorific values of jatropha, neem, cotton
Cetane number and their blends. The heating values are consistent with
the ASTM values for jatropha, cotton, neem and blends.
B5 B10 B15 B20 B25 B30 B100
These also match up with the work of Kaisan et al. (2017b)
Jatropha 58.474 57.9544 57.108 56.89 56.662 55.758 60.458
Neem 57.828 57.118 56.662 55.984 55.31 54.862 48.852 and Atabani and Cesar (2014). This makes them apt for
Cotton 58.242 57.576 57.088 56.89 56.436 55.758 57.8 consumption in diesel engine setups.
ASTM max 65 65 65 65 65 65 65
The acid values of biodiesel from jatropha and neem are
ASTM min 48 48 48 48 48 48 48
given in Table 7. According to Bozet al. (2009), the acid
ASTM: American society of testing of material.
value measures the amount of unreacted acid in the fin-
ished fuel, and is always an indication of oxidized fuel. A
Table 11. Total sulfur content of biodiesels and blends. high acid value damages fuel pumps and fuel filters. The
Total sulfur (% wt) acid values found in this study are very low; in fact, the
B5 B10 B15 B20 B25 B30 B100 acid values are even lower than the ASTM maximum stand-
Jatropha 0.192 0.183 0.170 0.155 0.141 0.129 0.048 ard which is 0.5. This implies that the fuels are good for
Neem 0.190 0.178 0.166 0.150 0.138 0.120 0.041 use in CI engines without any fear of damage to fuel
Cotton 0.192 0.181 0.168 0.153 0.139 0.126 0.049
ASTM max 0.05 0.05 0.05 0.05 0.05 0.05 0.05
pumps and filters.
ASTM: American society of testing of material.
Flash point is a degree of the temperature to which a
fuel must be heated such that the mix of air and vapor
above the fuel can be burned. Table 8 presents the flash
Table 12. Analyses of variance for specific gravity. points of biodiesel from jatropha, neem and cotton and
Criteria Sum of squares df Mean square F Sig. blends. The samples fall within ASTM standard values for
Between groups 0.001 3 0.000 1.179 0.338 flash points of biodiesels. This indicates that all the fuel
Within groups 0.006 24 0.000
samples are safe to handle. This is consistent with the work
Total 0.007 27
of Ewerenmadu et al. (2014) and Kaisan et al. (2017b).
10 M. KAISAN ET AL.

Table 15. Analyses of variance for pour point. Results

Criteria Sum of squares df Mean square F Sig. From the Table 12, the value of P is 0.338, which is
Between groups 26.571 3 8.857 .961 0.427 greater than 0.05, so the case of H0 is applicable and it
Within groups 221.143 24 9.214
Total 247.714 27
may be concluded that there is no significant difference
among the four categories of specific gravity. Hence the
four categories contribute equally and no further analysis
Table 16. Analyses of variance for cloud points. is needed.
Criteria Sum of squares Difference Mean square F Sig.
Between groups 26.679 3 8.893 0.675 0.576
Within groups 316.286 24 13.179
Total 342.964 27 Viscosity
Results
From the Table 13, it can be seen that the value of P is
Table 17. Analyses of variance for sulfur content.
0.359, and thus the same conclusions can be drawn as in
Criteria Sum of squares Difference Mean square F Sig.
the previous section.
Between groups .005 3 0.002 0.810 0.501
Within groups .046 24 0.002
Total .050 27
Acid value
Hypothesis
Based on the information presented in Table 9, it can This is based on the following two criteria:
be seen that the pour points of all the fuel samples con-
form to the ASTM standards. This means that the fuel sam-  H0: There is no significant difference between the
ples under investigation have a very good fluidity, do not five categories of acid value.
easily turn to gel and can be used at the lowest ASTM tem-  H1: There is a significant difference between the five
perature of 15
C without any trouble. These results are categories of acid value.
consistent with the findings of Kaisan et al. (2017a).
A fuel with a higher cetane number has a lower delay The level of significance, test statistic factor and decision
period and improved engine performance (Kaisan et al. criteria are taken to be the same as discussed in the previ-
2017b). Table 10 displays the cetane number of jatropha, ous section.
neem, cotton and blends. All the fuel samples are consist-
ent with the ASTM standards in terms of cetane number. Deduction
The total sulfur present in the biodiesel from jatropha From the Table 14, the value of P is 0.000, which is less
and neem is shown in Table 11 and is within the ASTM than 0.05, so the criterion H0 is rejected and it may be con-
limits. The reduction in sulfur content of the fuel reduces cluded that there is a significant difference between the
the tendency to emit sulfur (IV) oxide to the atmosphere five categories of acid values. Hence further experimenta-
during the combustion of the biodiesel fuel. These results tion is needed to determine their contributions using
are consistent with the findings of Kaisan et al. (2013) on Duncan’s multiple test.
sulfur content of wild grape seed biodiesel. It can be concluded that jatropha contributes more sig-
nificantly than all the neem variables, with a value
of 0.3929.
Analyses of variance for the physico-chemical properties
Table 12–17 provides over view of physicochemical proper-
ties of biodiesels and blends. Pour point
Hypothesis
The following hypotheses are applicable:
Specific gravity
Hypothesis
 H0: There is no significant difference between the
This is based on the following two criteria:
five categories of pour point.
 H1: There is a significant difference between the five
 H0: There is no significant difference between the
categories of pour point.
four categories of specific gravity.
 H1: There is a significant difference between the four
The level of significance, test statistics and decision cri-
categories of specific gravity.
teria are the same as those discussed in the previ-
ous section.
The level of significance (a) is taken to be 0.05.
The test statistics factor (F) is taken as a ratio of mean
Results
square ratio (MSR) and mean square equivalence (MSE):
From the Table 15 it can be seen that the value of P is
MSR 0.427, which is higher than 0.05; therefore, H0 and is
F¼
MSE accepted and it may be concluded that there is no signifi-
The decision criterion is based on the follow- cant difference between the five categories of pour point.
ing statement: Hence, no further tests are required and this implies that
H0 is rejected if the value of P is less than 0.05. the four categories contribute equally.
 BIOFUELS 11

Cloud point Disclosure statement

Hypothesis No potential conflict of interest was reported by the authors.
H0: There is no significant difference between the five
categories of cloud point.
H1: There is a significant difference between the five cat- ORCID
egories of cloud point. M.U. Kaisan http://orcid.org/0000-0003-4043-4682
The level of significance, test statistics and decision cri- S. Abubakar http://orcid.org/0000-0001-5659-8628
teria are the same as those discussed in the previ- S. Narayan http://orcid.org/0000-0001-7033-6341
ous section.

Results
From the Table 16 the value of P is 0.576, which is
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