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Analytical characterization of the Aegle marmelos pyrolysis products and

investigation on the suitability of bio‐oil as a third generation bio‐fuel for C.I
engine

Article in Environmental Progress & Sustainable Energy · December 2018

DOI: 10.1002/ep.13116

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Analytical Characterization of the Aegle marmelos
Pyrolysis Products and Investigation on the
Suitability of Bio-Oil as a Third
Generation Bio-Fuel for C.I Engine
P. Baranitharan, a K. Ramesh,a and R. Sakthivelb
a
Department of Mechanical engineering, Government College of Technology, Coimbatore, 641013, India;
[email protected] (for correspondence)
b
Department of Mechanical engineering, Amrita School of Engineering, Coimbatore, Amrita Vishwa Vidyapeetham, India
Published online 00 Month 2018 in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ep.13116

The present investigation emphasis on characteristics of harmful to the environment, renewability, availability, and bio-
pyrolysis products was obtained by intermediate pyrolysis of degradability [5]. Bio-oil derived from biomass can be used in
Aegle marmelos (AM) deoiled seed cake and appropriateness C.I engine fuel instead of fossil fuels without any C.I engine
of engine adaptation. The superior volatile matter (73.69%) modification [6]. Bio-oil obtained from waste biomass attains
contented AM biomass was elected as the feed stock in this the greater attention of biofuel researchers in an earlier decade
study. Pyrolysis experiment was done by a fixed bed reactor at [7]. Based on Indian biofuel policy 2017, it was suggested that
600 C and obtained 42–55% bio-oil yield. Investigation of about 20% of biofuel can be blended with fossil fuel [8]. The
bio-oil by GC/MS and FTIR established the occurrence of nonedible oils, fish oils, oils processing wastes, and animal fats
methyl, ester, alkanes, ketones and oxygenated chemicals have can be used as a feed stock material for bio-fuel productions
been alternates for fossil fuels. SEM and EDX analysis of bio- [9]. In the pyrolysis process, biomass is degraded in an inert
char exposes activated carbon and ensured that biochar can atmosphere which in turn generates bio-oil, bio-char, and syn-
be used in the waste water treatment plant, solid fuel, organic gas as main products [10,11]. Bio-oil derived from the pyrolysis
fertilizer, and natural mosquito destroyer. According to GC process having a higher amount of organics and can be
analysis, the presence of CH4, H2, and C2H6 evolved syngas in straight away used as a fuel in boilers and furnace usages. Bio-
AM pyrolysis process can be used C.I engines at dual fuel char can be used in various fields like organic fertilizers, chem-
mode operation. An engine test reveals that adding of the ical manufacturing, and solid fuels [2]. Syngas comprises the
pyrolysis oil diminished BTE (%) and increasing BSEC volatile organic components of CH4, CO2, H2, N2, it can be uti-
(MJ/kWhr). However, increasing bio-oil ratio blend with diesel lized in power source to reactors and industries [12].
reduces hazardous emissions like CO, HC, NOx, and smoke in Aegle marmelos tree comes under the family of rutacee [5].
the exhaust. Based on engine results, it was proposed that It is sacred tree innate to India which is seen generally in Lord
equal to 20% of AM bio-oil can be used as a fuel substitute for Shiva temples. The AM seeds are stable in a thick gummy pulp
diesel engines. © 2018 American Institute of Chemical Engineers (more than 50 seeds in a fruit) [13]. Aegle marmelos seeds
Environ Prog, 2018 were collected from AM fruits and the raw vegetable oil is
Keywords: AM seed cake, EDX, GC/MS, FTIR, engine test extracted by the mechanical press [14]. According to the
numerous literature reviews, not at all significant research has
INTRODUCTION
been done in AM pyrolysis products. Many researchers carried
Based on the BP review 2016, the consumption rate of out pyrolysis of various biomasses like sesame [15], Calophyl-
renewable energy was increased by 338.58% in 2015 [1]. In the lum inophyllum [2], prosopisjuliflora [16], sorghum [17], soy-
present world, the population was ever increasing dramatically bean [18], and ground nut [19] deoiled cakes.
which in turnincreasing the energy demand [2]. Huge This research to focus on the characteristics of AM seed
cake pyrolysis products valorization and investigated the possi-
researches are focused in fossil fuel-based bio-oil research. As
ble of AM pyrolysis oil as a diesel engine fuel. The intermedi-
the present energy requirements are inevitable. In the year
ate pyrolysis of AM seed cake was carried out in 2 kg fixed
2030, energy consumption rate of the Asia Pacific zone is
bed pyrolysis reactor at a temperature of 600 C and heating
expected to be increased up to 1.5% [3]. Biofuel reduces the
rate of 10 C/min in which higher pyrolysis oil yield was identi-
global warming rate by adopting a closed carbon cycle [4].
fied. Quantity and quality of the pyrolysis products yield are
Importantbenefits of biofuels are nontoxic, eco-friendly, not strongly based on biomass characteristics and the processing
conditions [20]. However, the pyrolysis oil blends were tested
Additional Supporting Information may be found in the online ver- in C.I engine and the engine operating parameters were stud-
sion of this article. ied. AM biomass and bio-char characterized using proximate
© 2018 American Institute of Chemical Engineers and ultimate analysis, SEM, FTIR, and EDX analysis. The AM

Environmental Progress & Sustainable Energy DOI 10.1002/ep 1

bio-oil characterized through physicochemical characteristics, Table 1. Testing conditions of GC–MS.
GC/MS and FTIR investigation. The third pyrolysis product
syngas was analyzed by using gas chromatography Sl. Thermo GC-Trace,
(GC) method. The most important benefits of this research No. Equipment used in GC–MS Thermo MS DSQ II
were to characterize the AM pyrolysis products are to find out
1 Gas chromatography
the correct applications toward commercialization in the suit-
conditions
able market. 2 Injection mode Split less
3 Carrier gas 99.99% pure Helium
MATERIALS AND METHODS 4 Column oven temperature 75 C
5 Injection temperature 250 C
Biomass Material 6 Column flow 1.0 mL/min
Figure 1 shows the AM de-oiled seed cake utilized in this 7 Progress of column oven
investigation. The AM seed cake was bought from neighbor- temperature
hood traders at a cost of Rs.7/kg. As per processing step, AM 8 Rate Temperature  C
seed cake was dried out in daylight to remove the moisture 9 - 75
content present in the feed stock. 10 10 260
11 Column: DB 35-MS Capillary
standard Non-Polar column
Pyrolysis Products Characterization 12 Film thickness (μm) 0.25
Proximate Analysis and Ultimate Study 13 Length (m) 30
Volatile matter (VM), moisture content (MC), fixed carbon 14 Diameter (mm) 0.25
(FC), and ash content (AC) of the AM biomass and bio-char 15 Mass spectrometry conditions
attained from this analysis adherence to ASTM D3172-07a by 16 Library NIST 11 and WILEY
PerkinElmer 2400 elemental analyzer. 17 Ion source temperature 220 C
The ultimate analysis gives information about the elemental 18 Start 50 m/z
composition of the sample material. It was performed using 19 End 650 m/z
Perkin Elmer elemental analyzer which determining the per-
centage of C, H, N, S, and O present in the sample material.
Gas Chromatography Coupled with Mass Spectrometry
Study
Fourier Transformer-Infra Red Spectroscopy Study Gas chromatography coupled with mass spectrometry
Fourier Transformer-Infra Red spectrometer analysis the (GC/MS) analysis was carried out by Thermo Trace Ultra GC
functional groups and molecules existed in the pyrolysis prod- system to identify the different organic compounds existent
ucts. FTIR analysis was done by PerkinElmer Spectrum FTIR in the pyrolysis oil. GC/MS study was done by as per
SP 10S/W (Model L160000E) spectroscopy and the absorption ASTMD4128-06 (2012). The identified components were com-
frequency range of the equipment was 400–4000 cm−1 with a pared with NIST and WLEY mass spectra library. The specifica-
resolution of 4 cm−1. tion and testing conditions of the GC/MS equipment are given
in Table 1.
Fuel Properties
SEM and EDX Analysis
The physical and chemical characteristics of AM bio-oil
were obtained as per ASTM standards. Physicochemical prop- Scanning Electron Microscopy (SEM) and Energy Dispersive
erties of the obtained pyrolysis bio-oil are very important char- X-ray spectroscopy analysis (EDX) gives the information about
acteristics because of this properties influence the usage of surface morphology, pore structure, shape and size ofthe sam-
engine application and toward the commercialization of the ples. SEM and EDX images obtained from JEOL (JSM-6480 LV)
pyrolysis oil. microscope on 6587 EDX scanning spectrometry detector hav-
ing acceleration voltage of 10 kV.

Gas Chromatography Analysis

In AM pyrolysis process the evolved syngas was analyzed
through GC (Gas Chromatography) by Shimadzu GC-2014 gas
analyzer. The evolved pyrolytic gas initially passed through
the silica filer fitted gas flow path finally collected the gas
bleeder. This syngas collected bladder was employed for the
gas chromatography analysis.

Engine Testing
Direct injection single cylinder C.I engine incorporated with
electrical loading was used for in this study. Testing of pyroly-
sis oil/diesel blends in a diesel engine is one of the major mile-
stones in the valorization of the pyrolysis products. A diesel
engine test rig was attached with AVL 250 MDS system and
AVL smoke meter to examine the emission composition while
operated with bio-oil. The C.I engine test was performed at
standard operating conditions. In this study, binary blends of
pyrolysis oil were analyzed (A10 [+10% AM bio-oil +90% die-
Figure 1. Aegle marmelos deoiled seed cake. [Color figure sel], A15 [15% AM bio-oil + 85% diesel], A20 [20% AM bio-oil +
can be viewed at wileyonlinelibrary.com] 80% diesel]). Owing to the dissimilarity in viscosity between
the bio-oil and diesel, it becomes unavoidable to emulsify the

2 Environmental Progress & Sustainable Energy DOI 10.1002/ep

Table 2. C.I engine specifications. reaction evolved pyrolytic gas was condensed by a shell and
water tube-cooled condenser arrangement.
Sl.No Specifications Primarily the pyrolysis reactor was cleaned appropriately to
ensure no char produced by the preceding study. Pyrolysis
1 Make Kirloskar Co. Ltd reactor outlet tube was joined with water tube-cooled con-
2 Type of injection Direct injection denser. Inside the reactor core 2 kg of AM seed cake was filled
3 Engine speed 1500 rpm and the reactor is sealed with a gasket. The gasket was to
4 Injection timing 23 bTDC ensure the inert atmosphere for the pyrolysis process. Pyrolysis
5 Cooling system Water cooling temperature was monitored continuously with the help of a
6 Number of stroke One PID controller. The reactor heating rate was varied through
7 Number of Cylinder Four dimmer stat, and the prerequisite temperature of 600 C was
8 Cylinder stroke 110 mm set in the PIDC panel. Once the pyrolysis reaction begins, the
9 Cylinder bore 87.5 mm evolved gas was passed over the condenser set-up. The con-
10 Rated output 3.5 kW densable portion of the gas got collected in the pyrolysis oil
11 Compression ratio 17.5:1 flask, whereas the noncondensable syngas was acquired in the
gas bladder for gas composition analysis. At the end of the
pyrolysis process remaining by-product of bio-char was
bio-oil with diesel fuel. Surfactants (Span-80 and Tween-80) removed after cooling of the reactor in the air.
are employed to emulsify the bio-oil blends. After completion
of emulsification blended fuels, the engine testing was carried
out in triplicate. The specification of C.I engine specification is Uncertainty Study of the Instruments
shown in Table 2. Table 3 shows the instruments detailed and uncertainty
analysis of this work. The uncertainty and errors of the instru-
ments are according to the working condition, instrument
Experimental Set-up for the Pyrolysis Process selection, calibration, and observation [21]. In the results of the
Aegle marmelos pyrolysis products were derived from inter- instruments, the doubt of the accuracy is referred to uncer-
mediate pyrolysis performed in 2 kg fixed bed reactor. This tainty. Uncertainty analysis was done by calculating variances
reactor was fabricated by SS 310 grade material, owing to the among the mean value at a level of 95% confidence level. All
extreme operating temperatures during the pyrolysis. The SS the experimentations were carried out by at least three times
310 grade material can withstand temperature up to 1000 C. and the observed values were averaged, to guarantee the reli-
The reactor is fitted with top feeding facilities and 20 cm inner ability and decrease the uncertainty level of the corresponding
dia was equipped with an electrical heater (240 V/9.5 A) and instrument. The overall uncertainty of the instruments falls
the reactor temperature was regulated by a PID controller inte- with the limit of 3, it is depicted that trust worthiness of mea-
grated with a K-type thermocouple. During the pyrolysis suring instruments performance [22].

Table 3. Instruments particulars and Uncertainty analysis.

Sl.
No. Instruments used Parameters measured Accuracy Uncertainty
1 Elemental analyzer-PerkinElmer 2400 Analyze the weight percentage of C,N,H, 0.3% 0.40
Series III O, and S in the sample
2 FT-IR SP10S/W Spectrometry-PerkinElmer Analyze the functional group present in 0.1 cm−1 0.006
Spectrum (Model L160000E) the samples (Wavelength in cm−1)
3 Gas chromatography–Mass spectrometry Analyze the organic compounds present 0.5% 0.17
(MS DSQ II mass selective detector) in the sample in area
4 Kinematic viscometer To determine the kinematic viscosity of <3% of 1.28
the sample (centistoke) measured
value
5 Density meter To determine the density of the sample 0.01 g/cm3 0.28
(g/cm3)
6 Bomb calorimeter To determine the calorific value of the 0.05% 1.23
sample (MJ/kg)
7 Pensky Martens apparatus To determine the flash point of the 2 C 1.68
sample ( C)
8 To determine the fire point of the sample 2 C 1.68
( C)
9 Sulfur content To determine the sulfur content of the 0.02 1.18
sample
10 Gas chromatography Analyze the gas composition of the 0.5% 1.96
sample (area %)
11 K-type Thermocouple To determine the pyrolysis reactor 1 C 0.1
temperature in  C
12 Diesel engine test rig Brake thermal efficiency 0.5% 0.05
13 Brake specific energy consumption 0.05 MJ/kWh 1
14 AVL smoke meter-Emission testing CO 0.01 vol % 2
15 CO2 0.03 vol % 0.5
16 HC 1 PPM 2
17 NOX 1 PPM 2
18 Smoke opacity 0.1% 1.25

Environmental Progress & Sustainable Energy DOI 10.1002/ep 3

Table 4. Elemental analysis of AM bio-mass. and phenols compounds [23]. The wave band between 3000
and 3100 cm−1 denotes the alkyl organic compounds [24]. The
Sl.No. Proximate analysis* Weight % broad of C-H stretch at 2840–3000 cm−1 exhibit the alkene.
The occurrence of α, β unsaturated ester group specifies the
1 Moisture content 3.01 absorbance frequency of C O stretching between
2 Ash 2.19 1715–1730 cm−1. Robust C C frequencies detected the range
3 Volatile 73.69 of 1662–1626 cm−1 considered the occurrence of alkene
4 Fixed carbon 21.11 group. The existence of C C stretch at 1566–1650 cm−1
Ultimate analysis* Wt % depicts the occurrence of cyclic alkene group [25]. The nitro
1 Carbon (C) 40.0497 compound N-O bending wave band was detected at
2 Hydrogen (H) 6.1474 1500–1550 cm−1 and C H bending between the frequencies
3 Oxygen (O) 52.2853 of 1380–1385 cm−1 designates the alkane [26]. The wave
4 Nitrogen (N) 1.4732 ranges from 400 to 1500 cm−1 is known as fingerprint region
5 Sulfur (S) 0.0005 where the wave frequencies are heavily occupied. The fre-
6 H/C molar ratio 1.67 quencies between 1163 and 1210 cm−1 reveal the presence of
7 O/C molar ratio 0.76 ester [27]. The spectrum analysis of alkene group by C C
8 Calorific value (MJ/kg) 20.17 bending band between 665 and 730 cm−1 [28]. In the spectrum
region of 1465 cm−1 shown the occurrence of alkane methy-
*Dry basis. lene compound by C H bending and it was noteworthy that
this region was the starting point of the fingerprint region. The
peak at 1247.12 cm−1 specifies the presence of ether (C O
bending). The C H bending region of 1450–1375 cm−1
RESULT AND DISCUSSION exposes the methyl group. The stretching vibration (C H) at
the end of the fingerprint region elucidates the existence of
Characterization of Pyrolysis Products vinyl ether.
Elemental Analysis of AM Biomass
Table 4 illustrates the results of proximate and ultimate
analysis of AM biomass. The augmented VM (73.69%) and a Physical and Chemical Properties of AM Bio-Oil
minimum value of FC (21.11%) confirm the suitability of AM The physicochemical properties of diesel and bio-oil are
cake for thermo chemical conversion and accomplished of given in Table 6. The maximum value of fire and flash points
producing a higher quantity of pyrolysis oil. The VM in the equate with neat diesel specifies that pyrolysis oil is safe dur-
biomass was disintegrated into organic vapors during pyroly- ing transit. In general, bio-oil is higher viscous which produces
sis. The lower value of MC (3.01%) and AC (2.19%) in feed the maximum difficulties of fuel spray and injection in engine
stock material depicts that AM seed cake can be employed as operation. This is can be rectified by up gradation techniques
low grade solid fuels [2]. The ultimate analysis conducted by such as esterification, emulsification, and hydro deoxygen-
as per ASTM D5291-96 and reveals that the feedstock is com- ation. Subsequently decreasing the viscosity of the pyrolysis
posed of carbon (40.0497%), hydrogen (6.1474%), oxygen oil using one of the mentioned methods, it can be used as a
(52.2853%), nitrogen (1.4732%), and sulfur (0.0005%). Reduced blend with diesel, which eventually decreases the diesel deple-
H/C and O/C molar ratio and fair calorific value confirm the tion. As compared to diesel, the calorific value of bio-oil is
suitability of the feedstock to be used as solid fuel. low, where as it can be compensated when blended with neat
diesel. Sulfur of the bio-oil is lower as compared with diesel,
which is lead to influential factor for SO2 emission. In this
FTIR Analysis of AM Pyrolysis Products regard, if AM bio-oil is used as engine fuel in C.I engines, it
Figure 2 shows the FTIR spectra of AM pyrolysis products. emits the lower amounts of sulfur oxide which decline the acid
Table 5 shows the organic functional compounds existent in rain level, atmosphere heat, and rate of global warming.
the AM pyrolysis products. The FTIR study spectacles the
pyrolysis products contain amines, alkanes, alkyl, ester, and
methyl compounds which are very important components of GC/MS Analysis of AM Bio-Oil
bio-fuel. The N-H stretching between 3500 and 3700 cm−1 rep- Table 7 shows the result of AM bio-oil analytical characteri-
resents the amines compounds. The wide O-H stretching zation through GC/MS. The GC/MS analysis acknowledged
between 3300 and 3400 cm−1 shows the presence of alcohols variant of organic compounds such as phenols, fatty acids,

Figure 2. FT-IR spectrum of AM pyrolysis products. [Color figure can be viewed at wileyonlinelibrary.com]

4 Environmental Progress & Sustainable Energy DOI 10.1002/ep

Table 5. FT-IR absorption frequencies of AM pyrolysis an ant-tumor agent. Benzene methanol is mostly used by a sol-
products. vent in wax and painting productions and addition up to 5% in
a lotion and shampoo as an active ingredient. Based on the
Absorption GC/MS results of AM pyrolysis oil contains rich fuel groups,
frequency Functional which is lead to efficiently used as an alternative engine fuel
(cm−1) groups Compounds or fuel additive.
3500–3700 N H stretching Amines SEM Analysis of Biomass and Bio-Char
3300–3400 O H stretching Aliphatic primary
Figure 3A,B represent the SEM images of biomass and bio-
amine
char, and it was evidenced by cracks of bio-char structure com-
3000–3100 C H stretching Alkene
pare to biomass structure. SEM analysis gives information about
2840–3000 C H stretching Alkane
the surface morphology of the biomass and bio-char. The SEM
1715–1730 C O stretching α,β-unsaturated ester
analysis of bio-char indicates the primary shrinkage causes due
1600–1650 C C stretching conjugated alkane
to the removal of moisture content and secondary defragmenta-
1626–1662 C C stretching Alkane
tion caused by devolatilization initiated the cracks owing to the
1566–1650 C C stretching Cyclic alkene
pyrolysis process. The level of structure breaking increasing
1500–1550 N O stretching Nitro compound
depends on the increase of the pyrolysis temperature.
1465 C H bending Methylene group
1450–1375 C H bending Methyl group
1380–1385 C H bending Alkane EDX Analysis of Biomass and Bio-Char
1200–1275 C O stretching Alkyl aryl Ester Figures 3(1,2) represent the EDX spectrum of AM biomass
1163–1210 C O stretching Ester and bio-char. Biomass has higher carbon content and lower
1020–1075 C O stretching Vinyl Ether potassium content. According to the EDX analysis of AM bio-
665–730 C C bending Alkene mass shows that maximum weight percentage of carbon
(66.6 wt %), oxygen (31.24 wt %), and minimum amount of cal-
cium (1.09 wt %) and potassium (1.07 wt %). However, bio-char
has higher carbon content (71.18 wt %). The higher amount of
esters, and alkanes with respect to RT (retention time). carbon present in bio-char favors the utilization of pollution-free
The highest area percentage (11.67%) was observed for solid fuel in the furnace [2], production of activated carbon, car-
1,2-Ethanediol, 1,2-diphenyl at RT of 6.47 min. Ethanediol is bon Nanotube manufacturing, the separator of heavy metal
commonly used as a freezing agent and in polyester fiber pro- dyes, natural mosquito coil, and aroma agarpathis [28]. The
duction. 10, 13-Eicosadienoic acid, methyl ester (linoleic acid maximum amount of carbon present in the AM bio-char which
methyl ester) was detected at the RT of 25.31 min with the attributed to the efficient carbonization of biomass at 600 C.
area of 5.89%. It is mainly used in medical, cosmetic and food Owing to the occurrence of a wide range of minerals (magne-
industries. Hexadecane nitrile was establishing with 5.80% area sium (0.34 wt %), phosphorus (0.65 wt %), potassium (1.15 wt
at RT of 21.83 min. Ethanol, 2-(hexadecyloxy) was observed %) and calcium (2.59 wt %)) in the bio-char, it can be used as
with the area of 4.98% at RT of 27.8 min. Ethanol compound is organic fertilizer in the agricultural field [29].
used mainly in medical usages (antiseptic, antidote, and etha-
nol is existing in more than 600 medicines production like GC Analysis of Syngas
acetaminophen, furosemide, phenobarbital, cough medicine, Among the syngas composition, carbon dioxide (CO2) was
ranitidine, and iron supplements. The main benefit of ethanol found in a large percentage (11.684%of concentration). The ther-
was used as a bio-fuel or bio-fuel additives. The pyrazine, mal decomposition of C O and COOH compounds evolved
2-ethyl-6-methyl compound was sensed at the lower RT of the carbon dioxide. The second-highest percentage of gas present
5.37 min. With the area of 1.76%. The other significant com- in the syngas composition was CH4 (methane) (10.063%) in the
pounds are farnesol (RT 8.73 min., 3.64% area) and Benzene retention time of 4.423 min. CH4and ethane (C2H6) both gases are
methanol (RT of 6.12 min., 1.83% area). Farnesolis used as the highly flammable in nature. At higher pyrolysis temperature, the
organic pesticide of mites and owing to this anti-bacterial thermal collapse of benzyl and methoxyl compounds to produce
movement, and also used as a deodorant in cosmetic goods as the methane and the aromatic components dehydrogenation to
form the hydrogen group [31]. Syngas contains H2, CO, CH4, CO2,
and C2H6 types of gas composition, so it can be used in power the
Table 6. Physical and chemical properties of AM pyrolysis oil reactor [12]. The advantages of syngas usage were reduced emis-
and diesel. sion compare to diesel fuel [32]. The AM syngas composition it
can be used as an alternate gas in S.I and C.I engines at dual fuel
AM mode modified engines.
ASTM pyrolysis
Property Units standards oil Diesel Effect of Temperature on AM Pyrolysis Products Yield
Calorific MJ/kg D240 41.35 45.40 Huge researchers investigated the influence on temperature
value on pyrolysis products yield and accomplish the optimal pyrol-
Kinematic Cst@40 C D445 7.83 3.49 ysis temperature for at higher bio-oil yield extraction. Bertero
viscosity et al. observed that the most favorable temperature of 550 C
Density kg/ for pyrolysis of channar and palm yielded up to 35–50% of
m3@30 C D4052 1.055 0.845 bio-oil [33]. Jackfruit peel pyrolysis process conducted at
Flash point 
C D93 79.12 65.57 550 C resulted in 32–50% of bio-oil [34]. Bordolai et al.
Fire point, 
C D93 52–98 74–105 observed that optimal pyrolysis temperature of 550 C during
Cetane – D613 42.65 50.06 the pyrolysis process of Pongamia glabra seed cover and
number attained the optimal bio-oil yield was 28.50% [35]. Ki et al.
pH pH E70 4.71 – derived the higher amount of pyrolysis bio-crude oil at the
Water wt % D1744 23.60 – pyrolysis temperature of 525 C for cassava peel (51.2%) [36].
content The consequence of pyrolysis temperature on AM pyrolysis
products is shown in Figure 4. While the pyrolysis temperature is

Environmental Progress & Sustainable Energy DOI 10.1002/ep 5

Table 7. GC–MS analysis of AM pyrolysis oil.

RT Area
(min) Compounds Mf Mw Area (%)
5.37 Pyrazine, 2-ethyl-6-methyl C7H10N2 122 329,629.1 1.76
6.12 Benzenemethanol C7H80 108 342,650.5 1.83
6.47 1,2-Ethanediol, 1,2-diphenyl C14H14O2 214 2,186,111. 11.67
7.57 Phenol, 2-[(dimethylamino)methyl]-4-ethyl C11H17NO 179 658,050.4 3.51
7.87 2-ISOPROPYLPYRIMIDINE C7H10N2 122 682,608.3 3.64
8.22 2-(2-Isopropenyl-5-methyl-cyclopentyl)-acetamide C11H19NO 181 318,477.4 1.70
8.73 Farnesol C15H26O 222 682,465.9 3.64
9.44 Benzeneethanamine, 2,5-dimethoxy-à-methyl C11H17NO2 195 493,600.4 2.64
9.77 m-Aminophenylacetylene C8H7N 117 364,611.3 1.95
11.36 2-(1,2,3,4-Tetrahydronaphthalen-1-yl)ethyl methanesulfonate C13H18O3S 254 239,454.7 1.28
13.38 Eicosane, 10-methyl C21H44 296 254,863.6 1.36
à-D-MANNOFURANOSIDE, METHYL, CYCLIC 2,3:5,6-BIS
14.29 (ETHYLBORONATE) C11H20B2O6 270 245,095.3 1.31
Ethyl-3,4-dihydro-2-(1-hydroxypropyl)-6-methyl-2H-pyran-5
18.86 -carboxylate C12H20O4 228 288,030.9 1.54
19.12 10-Methyl-octadec-1-ene C19H38 266 341,292.0 1.82
20.28 1-methylethyl tetradecanoate C17H34O2 270 627,771.0 3.35
21.83 Hexadecanenitrile C16H31N 237 1,086,802. 5.80
22.30 Tridecanoic acid, 4,8,12-trimethyl-, methyl ester C17H34O2 270 277,679.6 1.48
23.11 Hexadecane, 2,6,10,14-tetramethyl C20H42 282 200,121.4 1.07
25.31 10,13-Eicosadienoic acid, methyl ester C21H38O2 322 1,102,889. 5.89
25.74 Octadecanenitrile C18H35N 265 418,121.2 2.23
2-(2-Chloro-2,3,3-trifluoro-cyclobutyl)-cyclopropane carboxylic acid
27.19 methyl ester C9H10ClF3O2 242 490,597.8 2.62
27.8 Ethanol, 2-(hexadecyloxy) C18H38O2 286 932,761.4 4.98
28.21 Bacteriochlorophyll-c-stearyl C52H72MgN4O4 840 293,483.7 1.57
29.86 Octadecane, 3-ethyl-5-(2-ethylbutyl) C26H54 366 694,893.4 3.71
30.22 2,2,3,3,4,4 HEXADEUTERO OCTADECANAL C18H30D6O 268 908,515.2 4.85
33.38 Cyclohexane, 1,3,5-trimethyl-2-octadecyl- C27H54 378 529,675.6 2.83
Methyl-2-(4,8-Diacetoxy-3-bromo-6-methoxy-9,10-dioxo-9,1
34.44 0-dihydroanthraquinon-2-ylmethyl) C29H27BrO12 646 242,240.8 1.29
3,5,7-Tris(trimethylsiloxy)-2-[3,4-di(trimethylsiloxy)
34.65 phenyl]-4H-1-benzopyran-4-one C30H50O7Si5 662 225,720.9 1.21
3,3,4,4-Tetracyano-6-phenyl-5-(p-tolyl)-2-(p-methox
36.28 yphenylimino)-2,3,4,5-tetrahydropyridine C29H20N6O 468 428,712.2 2.29

RT-Retention time Mw-Molecular weight Mf-Molecular formulae

increased from 500 to 650 C, a diminishing tendency in bio-char Brake Specific Energy Consumption (BSEC in MJ/kWhr)
yield was detected whereas syngas yield was augmented reason- The BSEC diminished with the rise in BMEP for all bio-oil
ably. The peak bio-oil yield was detected at 600 C after which is blends (Figure 6). At 100% load, BSEC values are 13.232,
gets decreased with augmentation in gaseous yield owing to the 12.8185, 11.578, and 16.54 MJ/kWhr for A10, A15, A20, and
secondary decomposition of bio-oil at a higher temperature. Dur- diesel, respectively. The lower BSEC was observed in A20
ing the pyrolysis process, increasing tendency in bio-oil yield blend, and also higher BSEC detected in diesel fuel. Reduced
accompanied by a reduction in bio-char yield was observed. The BSEC was observed for various pyrolysis oil blends at all load-
maximum yield of bio-oil was observed at 600 C, which is the ing conditions as compared with diesel, this is due to fuel
optimal temperature of AM pyrolysis process. emulsification, bio-oil blend with diesel and enriched oxygen
contents present in the AM bio-oil blends.

ENGINE ADAPTATION
Emission Characteristics of AM Bio-Oil
Performance Characteristics of AM Bio-Oil Carbon Mono Oxide
Brake Thermal Efficiency (BTE %) The comprehensive combustion of engine fuel is indicated
From Figure 5, the BTE rises linearly in proportion with by the amount of CO2 emission [38]. However, the inadequate
brake mean effective pressure (BMEP). It is evident that BTE combustion of the fuel indicated by the higher amount of CO
of different blended fuels was recorded higher than that of die- emission. Figure 7 spectacles the correlation between BMEP
sel fuel. A20 blend indicated the maximum BTE compared with respect to CO for various bio-oil blends. From the figure,
with other blends. At peak loading conditions, BTE for A10, it is illustrated that increasing BMEP, which shows the
A15, A20 and diesel was 25.18%, 26.62%, 29.67%, and 20.64% increases CO in the exhaust for entire test fuels and diesel. It is
respectively. The high oxygen contention bio-fuel enhance the significant that, bio-oil blends emit lower CO emission as com-
combustion process which leads to lower fuel consumption to pared to diesel traumatically. It is noteworthy that diesel exhib-
attain the necessary power output which in turn increases the ited the maximum CO at all loading condition as compared
BTE (%) [37]. with AM bio-oil blends. At peak load conditions A10, A15,

6 Environmental Progress & Sustainable Energy DOI 10.1002/ep

Figure 3. SEM micrograph and EDX spectrum of biomass and bio-char. [Color figure can be viewed at wileyonlinelibrary.com]

A20, and diesel indicated the CO emission of 0.32%, 0.29%, Oxides of Nitrogen
0.22%, and 0.34% of volume correspondingly. These results The variant of BMEP with oxides of nitrogen (NOx) repre-
indicate that AM pyrolysis oil is a suitable engine fuel in its sented in the Figure 9. Diesel engines NOx emission is mostly
place of diesel in C.I engine rendering to CO value and CO composed of nitric oxide (NO) with traces of nitrogen di-oxide
emission results confirm that AM bio-oil usage which dimin- (NO2). The NOx emission is based on the air and fuel mixture
ishes the toxic CO levels. ratio (NOx of promt), bio-oil /diesel opus (NOx of fuel) and
combustion temperature (NOx of thermal) [39]. Rendering to
Hydro Carbon the Zeldovich mechanism, NOx created at a higher tempera-
Figure 8 depicts the variant of BMEP and hydro carbon ture (around 1500 C) owing to the chemical reaction of O2and
(HC). During engine operation the inadequate combustion of N2molecules in the combustion chamber. From the figure,
fuel molecules results in HC emission [14]. The decreasing higher NOx of diesel and A10, A15, A20 were 1511, 1437,
trend in HC emission was detected in augmenting the BMEP 1498, and 1501 ppm, respectively, and growing the BMEP
for entire test fuels and neat diesel. The HC emission of A10, leads to maximize the NOx emission intensities at entire
A15, A20, and diesel were 84, 65, 58, and 99 ppm correspond- engine loads. The increase of NOx with loading may attribute
ingly at full engine load conditions. As compared with diesel to rising combustion temperature at high loads. The minimum
fuel, bio-oil blends emit a lower amount of HC, this is due to NOx in pyrolysis oil operation was detected by the quenching
the fact that enhance the poor spray, fuel injection and atomi- effect of moisture content in bio-oil which decreases flame
zation features of bio-oil bends. temperature, thus decreasing NOx. It is noteworthy that diesel
emits higher NOx emission as compared with AM bio-oil
blends, it is exposed that usage of AM pyrolysis oil blend in C.
I engine, reduce the harmful emission to the environment.

35

30

25 A10 blend
BTE (%)

20 A15 blend

A20 blend
15
DIESEL
10

0
1.06 2.06 3.06 4.4
BMEP (bar)

Figure 4. Effect of temperature on AM pyrolysis products Figure 5. Brake thermal efficiency. [Color figure can be
yield. [Color figure can be viewed at wileyonlinelibrary.com] viewed at wileyonlinelibrary.com]

Environmental Progress & Sustainable Energy DOI 10.1002/ep 7

 35 45
BSEC (MJ/kWhr) 30 40

25 35

Smoke opacity (%)

A10 blend
20 30
A15 blend A10 blend
15 A20 blend 25
A15 blend
DIESEL 20
10 A20 blend
15
5 DIESEL
10
0
1.06 2.06 3.06 4.4 5
BMEP (bar) 0
1.06 2.06 3.06 4.4
Figure 6. Brake specific energy consumption. [Color figure BMEP (bar)
can be viewed at wileyonlinelibrary.com]
Figure 10. Smoke opacity. [Color figure can be viewed at
wileyonlinelibrary.com]

0.5

0.4 Smoke Opacity

CO (Volume %)

A10 blend Figure 10 depicts the relationship between BMEP and

0.3 A15 blend smoke opacity at various engine loads. During the combus-
A20 blend
tion, exhaust smoke opacity depends upon the rich oxygen
0.2
content of the fuel [40]. At the full load condition, the smoke
DIESEL opacity for A10, A15, A20 blends, and diesel were 25%, 23%,
0.1
22%, and 28%, respectively. From the figure, it seems that ris-
0 ing BMEP diminishing smoke opacity in exhaust port for all
1.06 2.06 3.06 4.4 pyrolysis oil blends and diesel. It is noteworthy that diesel
BMEP (bar) emits highest smoke emission as compared to all AM bio-oil
blends. Among the bio-oil blends A10 showed the increased
Figure 7. Carbon monoxide. [Color figure can be viewed at smoke emission. Compare to diesel, AM bio-oil blends showed
wileyonlinelibrary.com] the reduction in smoke opacity due to sufficient oxygen pre-
sent in bio-oil which encourages soot oxidation thereby reduc-
ing the smoke opacity.

160 CONCLUSION

140
The pyrolysis temperature at 600 C was caused in a higher
amount of bio-oil yield of 42 to 55%. Physicochemical proper-
120
A10 blend ties, FTIR and GC/MS analyses results were indicated that AM
HC (ppm)

100 bio-oil contains hexadecane, pentadecane, octadecanenitri-

A15 blend
80 leare rich in the range of C13-C26 like diesel fraction and which
60 A20 blend indicate the AM bio-oil instead of fossil fuel. From the EDX
40 DIESEL analysis bio-char contains a higher amount of C, Mg, Ca, P,
20 and K which show that used as a solid fuel and organic fertil-
0
izer, which leads to reducing the soil acidity and improving
1.06 2.06 3.06 4.4 the soil quality. According to GC analysis, methane and ethane
have a high percentage of the composition. In general, meth-
BMEP (bar)
ane and ethane highly inflammable nature, which is used as
Figure 8. Hydro carbon. [Color figure can be viewed at an alternate energy source for modified engines. The ultimate
wileyonlinelibrary.com] application of the pyrolysis oil was engine operation. From the
engine test consequence was specified that bio-oil addition
augmented the BTE (%) and decreased the BSEC (MJ/kWhr)
when compared with base line diesel. It is noteworthy that,
emission behavior of AM pyrolysis oil depicts that superior
1800
result, which is a reduction in harmful CO, HC, and smoke
1600
opacity emission as compared with diesel. According to the
1400
engine investigation, it is evidently suggested that up to 20% of
1200
NOx (ppm)

A10 blend AM bio-oil can be emulsified with diesel and employed as an

1000 A15 blend engine fuel to attain enhanced engine operation.
800
A20 blend
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