C 26

Technical Note
Characterization of biochar and bio-oil samples obtained from carbonization

of various biomass materials
Didem O
zimen
*
, Ays egu l Ersoy-Meriboyu
Istanbul Technical University, ChemicalMetallurgical Engineering Faculty, Department of Chemical Engineering, Maslak 34469, Istanbul, Turkey
a r t i c l e i n f o
Article history:
Received 31 March 2009
Accepted 10 November 2009
Available online 22 December 2009
Keywords:
Biochar
Bio-oil
Apricot stone
Hazelnut shell
Grapeseed
Chestnut shell
a b s t r a c t
Apricot stone, hazelnut shell, grapeseed and chestnut shell are important biomass residues obtained
from the food processing industry in Turkey and they have a great importance as being a source of
energy. In this study, the characteristics of bio-oil and biochar samples obtained from the carbonization
of apricot stone, hazelnut shell, grapeseed and chestnut shell were investigated. It was found that the
biochar products can be characterized as carbon rich, high heating value and relatively pollution-free
potential solid biofuels. The bio-oil products were also presented as environmentally friendly green
biofuel candidates.
2009 Elsevier Ltd. All rights reserved.
1. Introduction
Renewable energy is a kind of energy produced from any source
that can be maintained in a constant supply over time. The most
important renewable energy sources can be classied as solar,
wind, hydro, geothermal, wave and biomass. Among these sources
the biomass is considered as an important one since it could be
suitable alternative for conventional fossil fuels.
Unlike solar, wind and hydroelectric systems, modern biomass
energy systems could be set up in virtually any location where
plants can be grown or domestic animals are reared. This is one of
the most important properties of the biomass energy in which it
differs from other renewable energy systems and it offers an
opportunity for sustainable energy. Among renewable energy
sources, biomass is the only energy source that can be used without
any energy storage systems. Using biomass can help reduce global
warming compared to a fossil fuel-powered plant. Plants use and
store CO
2
when they grow. CO
2
stored in the plant is released when
the plant material is burned or decays. By replanting the crops, the
newplants can use the CO
2
produced by the burned plants. So using
biomass and replanting helps close the carbon dioxide cycle.
However, if the crops are not replanted, then biomass can emit
carbon dioxide that will contribute toward global warming [1].
Biomass resources include various natural and derived mate-
rials, such as woody and herbaceous species, wood wastes, energy
crops, bagasse, agricultural and industrial residues, waste paper,
municipal solid waste, sawdust, biosolids, grass, waste from food
processing, animal wastes, aquatic plants and algae etc. [2].
Biomass sources can generally be dened as any carbohydrate
material which mainly consists of carbon, hydrogen, oxygen and
nitrogen. Some biomass types also carry signicant proportions of
inorganic species. The concentration of the ash arising from these
inorganics changes from less than 1% in softwoods to 15% in
herbaceous biomass and agricultural residues [2]. The chemical
structure and major organic components in biomass are extremely
important in the development of processes for producing derived
fuels and chemicals. The major organic components of biomass can
be classied as cellulose, hemicellulose and lignin [3].
Turkey has a rich agricultural biomass potential. Various agri-
cultural residues are available. One of the main important biomass
sources in Turkey is food processing industry wastes. Apricot stone,
hazelnut shell, grapeseed and chestnut shell are important biomass
residues obtained in Turkey and they have a great importance as
being a source of energy and they mostly are used to produce
energy for domestic purposes by direct combustion. Since this type
of usage is not economical, these biomass sources must be con-
verted into more useful forms by using different conversion
technologies.
In this study, the characteristics of biochar and bio-oil samples
acquired by carbonization of apricot stone, hazelnut shell,
* Corresponding author. Tel./fax: 90 212 518 3565.
E-mail address: didem.ozcimen@gmail.com (D. O
zimen).
Contents lists available at ScienceDirect
Renewable Energy
j ournal homepage: www. el sevi er. com/ l ocat e/ renene
0960-1481/$ see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.renene.2009.11.042
Renewable Energy 35 (2010) 13191324
grapeseed and chestnut shell were identied to evaluate the
feasibility of using them as alternative to conventional fossil fuels.
2. Experimental section
2.1. Materials
In the experimental study, the apricot stone (Prunus armeniaca)
obtained from Malatya located in the east anatolian region of
Turkey, the hazelnut shell (Corylus avellana) obtained from Giresun
located in the Black Sea region of Turkey, the grapeseed (Vitris
vinifera) obtained from a vine factory located in the middle
Anatolian region of Turkey and the chestnut shell (Castanea sativa
Mill) obtained froma chestnut candy factory in Bursa located in the
Marmara region of Turkey were used as biomass samples. All
biomass samples were initially ground and sieved to obtain the
particle size of 11.4 mm for apricot stone and hazelnut shell and
the average particle diameters of 0.657 mm and 0.377 mm, for
grapeseed and chestnut shell, respectively. After sieving air-dried
samples were kept in glass jars and used as necessary.
2.2. Carbonization of biomass samples
The carbonization experiments were performed in a Jenkner
type retort which is a cylindrical stainless steel xed bed reactor
with a length of 270 mm and an inner diameter of 130 mm. The
reactor was heated externally by an isolated electrical furnace
where temperature was measured by a NiCrNi thermocouple
inside the bed. During the carbonization the inner and outer
temperatures of the reactor were controlled continuously. Before
heating, the system was ushed with dry nitrogen for 30 min to
remove all traces of oxygen. After carbonization at nal tempera-
ture value, which lasted 30 min, the nal weight of samples was
determined to calculate the biochar and bio-oil yields.
In this study, the samples obtained at the carbonization condi-
tions, where the maximum biochar and bio-oil yields were
obtained were took into consideration for characterization. These
conditions as reported previously [46] for different biomass
samples were summarized in Table 1.
The maximum biochar yields for the conditions given in Table 1
were found as 34.65%, 51.53%, 52.98% and 58.80% for apricot stone,
hazelnut shell, grapeseed and chestnut shell samples, respectively.
The maximum bio-oil yields, on the other hand, were determined
for those conditions as 35.82%, 41.95%, 49.11% and 36.11% for apricot
stone, hazelnut shell, grapeseed and chestnut shell samples,
respectively.
2.3. Characterization of biomass, biochar and bio-oil samples
Characterization of original biomass, produced biochar and bio-
oil samples was performed by using various analysis methods. The
caloric values of samples were measured by the ASTM bomb
calorimeter method [7] using a IKA Calorimeter C 7000 model
instrument. The proximate analysis of biomass and biochar
samples was also done according to ASTM standards [810].
Physical properties of biomass and biochar samples such as
porosity, total pore volume and surface area were measured by
using an Quantachrome Autoscan-33 mercury intrusion poros-
imeter and Quantachrome NOVA 1200 model surface areameter.
SEM micrographs of biomass and biochar samples were taken by
using a Jeol Model JSMdT330 Scaning Electrone Microscope which
is operated at 20 kV. Fourier Transform Infrared (FTIR) spectro-
scopic analysis of all samples was performed using a PerkinElmer
Spectrum 1 model instrument. The GCMS analysis of the bio-oil
samples was carried out using a Clarus 500 GC instrument
(PerkinElmer) coupled to a Clarus 500 MS system (PerkinElmer).
Apolar capillary column (i.d.-BP
*
5, length:30 m, diameter:
0.25 mm) was used as MS column.
Table 1
The carbonization conditions where the maximum biochar and bio-oil yields were obtained for different biomass samples.
Carbonization conditions Biochar Bio-oil
Apricot stone Hazelnut shell Grapeseed Chestnut shell Apricot stone Hazelnut shell Grapeseed Chestnut shell
Heating rate (K/min) 5 5 5 5 20 20 20 20
Sweep gas owrate (cm
3
/min) 0 0 0 0 1000 1000 1000 1000
Temperature (K) 823 750 750 750 823 823 823 823
Particle diameter (mm) 11.4 11.4 0.657 0.377 0.2500.355 0.2500.355 0.657 0.377
Table 2
The gross caloric values of biomass, biochar and bio-oil samples.
Material Gross caloric value (MJ/kg)
Apricot stone 19.28
Hazelnut shell 18.33
Grapeseed 20.51
Chestnut shell 15.49
Apricot stone biochar 30.76
Hazelnut shell biochar 29.08
Grapeseed biochar 26.73
Chestnut shell biochar 25.86
Apricot stone bio-oil 22.72
Hazelnut shell bio-oil 26.79
Grapeseed bio-oil 29.76
Chestnut shell bio-oil 26.72
Table 3
The proximate analysis results of biomass and biochar samples (dry base).
Material Volatile matter (%) Fixed carbon (%) Ash (%)
Apricot stone 77.12 21.47 1.41
Hazelnut shell 71.67 26.51 1.83
Grapeseed 70.53 21.98 7.49
Chestnut shell 69.74 28.67 1.59
Apricot stone biochar 19.83 71.70 8.47
Hazelnut shell biochar 30.26 63.16 6.58
Grapeseed biochar 39.45 50.96 9.59
Chestnut shell biochar 34.32 60.32 5.36
Table 4
The physical properties of biomass and biochar samples.
Material Porosity (%) Total pore volume
(ml/g)
BET surface area
(m
2
/g)
Apricot stone 0.0241 0.0303 10.5299
Hazelnut shell 0.0463 0.0434 5.8421
Grapeseed 0.0630 0.0756 10.5881
Chestnut shell 0.2764 0.3281 7.0103
Apricot stone biochar 0.1309 0.1847 11.2474
Hazelnut shell biochar 0.1130 0.1250 14.6836
Grapeseed biochar 0.1316 0.1643 14.4770
Chestnut shell biochar 0.1702 0.1842 0.6717
D. O
zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1320

Fig. 1. Apricot stone and its biochar micrographs.
Fig. 2. Hazelnut shell and its biochar micrographs.
Fig. 3. Grapeseed and its biochar micrographs.
Fig. 4. Chestnut shell and its biochar micrographs.
D. O

3. Results and discussion
3.1. Comparison of fuel properties
Gross caloric values of the biomass, biochar and bio-oil
samples were given in Table 2.
As can be seen from the results given in Table 2, grapeseed has
the highest (20.51 MJ/kg) and the chestnut shell has the lowest
(15.49 MJ/kg) gross caloric values among all the biomass samples.
In comparison with biomass materials, their biochar and bio-oil
samples have higher gross caloric values. The highest gross calo-
ric values for biochar and bio-oil samples were found as 30.76 MJ/
kg for apricot stone biochar and 29.76 MJ/kg for grapeseed bio-oil.
The proximate analysis results of the biomass and biochar
samples were given in Table 3.
According to the proximate analysis results of biomass samples
given in Table 3, the volatile matter contents are changed between
the range of 69.74% and 77.12%. While chestnut shell has the lowest
volatile matter, the highest volatile matter was found for apricot
stone sample. The xed carbon contents of biomass samples are
changed between the range of 21.47% and 28.67%. Chestnut shell
has the highest xed carbon whereas apricot stone has the lowest
xed carbon among all biomass samples. The change interval of the
ash contents was determined between 1.41% and 7.49%. The highest
and lowest ash contents were found for grapeseed and apricot
stone samples, respectively.
In comparison with raw biomass samples, a decrease in volatile
matter and an increase in xed carbon content were observed for
biochar samples, as expected. The presence of volatile matter in
biochar samples shows incomplete thermal degradation during
carbonization The ash content of biochar samples is also found
higher than the biomass samples due to the mineral matter which
form ash remains in biochar after carbonization.
By comparison of the fuel properties given in Tables 2 and 3, the
biochar products can be characterized as carbon rich, high caloric
value and potential solid biofuels. The produced biochars can be
utilized in various industrial applications as an alternative to solid
fossil fuels. The bio-oil products can also be presented as biofuel
candidates due to their high caloric values.
3.2. Comparison of physical properties
Since the physical properties effect the combustion character-
istics of solid fuels [11] some of the physical properties of biomass
and biochar samples such as porosity, total pore volume and
surface area were determined and the results were given in Table 4.
The porosity values show that the porosity of biomass and
biochar samples change between 0.0240.276 (%) and 0.1130.170
(%), respectively.
As can be seen from Table 4, the BET surface areas of biomass
and biochar samples change between 5.842110.5881 (m
2
/g) and
0.671714.6836 (m
2
/g), respectively.
Porosity, total pore volume and BET surface area values of bio-
chars were found higher than their biomass samples except
chestnut shell biochar (Table 4). The difference observed in
chestnut shell biochar sample can be attributed to different phys-
ical appearance and shape of the raw material in comparison with
other biomass samples. Although, apricot stone, hazelnut shell and
grapeseed have a granular shape and appearance, the shape of
chestnut shell is resembling spongy in appearance.
Table 6
Functional groups of biochar samples determined by the FTIR analysis.
Wave numbers (cm
1
) Functional groups
Hazelnut shell biochar
3387 OH stretching
1577 Aromatic C]C ring stretching
1373 Aliphatic CH
3
deformation
1137 Aromatic CO stretching
1021 Aliphatic ether CO and alcohol CO stretching
869 1 adjacent H deformation
Apricot stone biochar
2972 Aliphatic CH stretching
1393 Aliphatic CH
3
deformation
Grapeseed biochar
Chestnut shell biochar
Table 5
The functional groups of biomass samples determined by the FTIR analysis.
Wave numbers (cm
1
) Functional groups
Hazelnut shell
2924 Aliphatic CH stretching vibration
1709 Aromatic carbonyl/carboxyl C]O stretching
1370 Aliphatical CH
3
deformation
Apricot stone
3342 OH stretching
1370 Aliphatic CH
3
deformation
897 Aromatic ring
Grapeseed
1317 Aliphatical CH
2
deformation
Chestnut shell
3324 OH stretching
1018 Aliphatical ether CO and alcohol CO stretching
D. O

SEMmicrographs of biomass and biochar samples were given in
Figs. 14. Scanning electron microscopy (SEM) is a potential tech-
nique for studying morphology of solid fuel particles. SEM analysis
has been especially used to evaluate the structural variations in
char particles after different thermal treatments.
SEMimages are very useful to obtain accurate details about pore
structure of biochars and the comparison between biochars and
their raw materials would then allow us to draw conclusions on
morphological changes during the carbonization stage.
It is obvious from the porosity and surface area values and the
SEM micrographs that the physical properties and the surface
morphology of biomass samples changed after carbonization.
Biochar samples enriched in carbon, contain several cracks and
holes formed because of the evolution of volatile matter during
carbonization. The extent of devolatilization has a signicant
effect on the characteristics of the produced biochar. As known,
higher volatile matter release produces biochars with lower
densities, higher porosities and signicantly different pore
structure [12].
It can be concluded from the physical properties (Table 4) and
SEM images (Figs. 14) of biochar samples, biochars have some
internal pores and cracks, while the pores of biomass samples not
distinctively found. Thus, it is possible to use the biochar samples as
a carbon feedstock for producing different carbon materials such as
activated carbon, carbon nanotubes and carbon bres.
3.3. Comparison of FTIR results
The functional groups that which were identied from the FTIR
spectrumof the biomass, biochar and bio-oil samples were given in
Tables 57.
The FTIR spectra were recorded in the transmission mode
between 4000 and 650 cm
1
for all samples. As can be seen from
the FTIR results given in Table 5, all original biomass samples have
similar aromatic and aliphatic functional groups. Table 6 presents
that, all biochar samples has also similar chemical groups. However,
there is an alteration in aromatic structure of biochar samples in
comparison with biomass samples. The peaks between 700 and
900 cm
1
corresponding to an aromatic CH stretching vibration
that indicates the presence of adjacent aromatic hydrogen in bio-
char samples is not seen in biomass samples [13]. As can be seen
from Table 7 all bio-oil samples have also similar chemical groups
as aromatic and aliphatic functional groups predominantly. The
peaks for bio-oil samples were determined particularly between
702 and 2932 cm
1
.
3.4. The GCMS and the column chromatography results of
bio-oil samples
The results of GCMS analysis of bio-oil samples were given in
Table 8.
Table 7
The functional groups of bio-oil samples determined by the FTIR analysis.
Wave numbers (cm
1
) Functional groups
Hazelnut shell bio-oil
1377 Aliphatic CH
3
deformation
1114 Ketone or ester bonding
736 4 adjacent aromatic H deformation
Apricot stone bio-oil
1393 Aliphatic CH
3
deformation
1266 Aromatic CO and phenolic OH stretching
930 Mono, polycyclic and branched aromatic groups
Grapeseed bio-oil
1463 Aliphatic CH deformation
Chestnut shell bio-oil
1367 Aliphatic CH
3
deformation
1112 Polycyclic heteroatoms
Table 8
GCMS chromatogram results of bio-oil samples.
Hydrocarbon species Retention time (min) Concentration (mg/g)
Apricot stone bio-oil
C
5
3.38 80
C
6
3.83 45
C
11
12.21 32.5
C
19
19.82 31
Hazelnut shell bio-oil
C
5
3.88 61.5
C
6
4.75 45
C
7
7.75 32.5
C
8
9.62 24.6
C
17
17.80 42
C
19
19.87 54.5
Grapeseed bio-oil
C
7
7.63 20.5
C
17
17.78 25.5
C
19
19.84 28
C
30
28.78 37
Chestnut shell bio-oil
C
5
3.44 24
C
6
6.76 20.1
C
7
9.59 32.5
C
11
16.57 36
C
16
17.79 39
C
17
18.52 26
C
19
20.18 19
C
24
27.12 26
C
28
28.46 30
Table 9
The results of column chromatographic fractionation of the bio-oil samples.
Fractions Yield (%)
Apricot stone
bio-oil
Hazelnut shell
bio-oil
Grapeseed
bio-oil
Chestnut shell
bio-oil
Asphaltane 37.75 38.40 28.50 40.53
n-Pentane solubles 62.25 61.60 71.50 59.47
n-Pentane solubles
n-Pentane eluate 15.60 16.50 14.10 16.20
Toluene eluate 41.50 40.65 42.75 41.10
Methanol eluate 42.90 42.85 43.15 42.70
D. O

The hydrocarbons present in bio-oil samples and their quanti-
ties were identied by GCMS technique. The most abundant
hydrocarbon distribution was observed in the range of C
5
C
19
chain
structure in both of apricot stone and hazelnut shell bio-oils and
their peak intensity are the same. The most abundant hydrocarbon
distribution was observed in the range of C
7
C
30
chain structure in
grapeseed bio-oil, while the peak intensity is in C
30
and the most
abundant hydrocarbon distribution was observed in the range of
C
5
C
28
in chestnut shell bio-oil, the peak intensity was C
16
for
chestnut shell bio-oil.
The bio-oil samples were also fractionated using column chro-
matography with a length of 50 cm and an inner diameter of 1 cm.
Glass wool was placed at the bottom of the column. The column
used was packed with silica gel 70230 mesh, pretreated at 600

C
for 8 h prior to use. The column chromatography procedure was
carried out for fractionation of bio-oil samples [14]. In this proce-
dure 1 g of bio-oil was weighed and held in n-pentane for one
night. Soluble fractions of oil in n-pentane and non-soluble frac-
tions of oil in n-pentane were separated by ltration. Then the
amount of non-soluble asphaltene was determined. From the oil
fraction that was soluble in n-pentane, n-pentane was removed by
rotary evaporator and the amount of oil fraction that was soluble in
n-pentane was found. The separated fraction, which was mixed
with silica gel was placed at the top of the column. 150 cm
3
of n-
pentane, 100 cm
3
of toluene and 100 cm
3
of methanol were added
respectively to produce aliphatic hydrocarbon, aromatic hydro-
carbon and polar fractions. The solvents of the each fraction were
removed in rotary evaporator and the amount of fraction was
calculated. The column chromatography results of the bio-oil
samples were summarized in Table 9.
Bio-oil samples were separated into two fractions according to
its pentane solubility as asphaltene and n-pentane solubles. Results
of the column chromatography of the bio-oil samples showed that
the apricot stone bio-oil consists of 37.5% asphaltenes and 62.25%
n-pentane solubles. Depending on the eluate yields, that can be
soluble fraction of oil in n-pentane 15.60% paranic, 41.50%
aromatic and 42.90% polar components were determined. As can be
seen in Table 9, chestnut shell bio-oil has the highest asphaltenes
content as 40.53% and grapeseed bio-oil has the highest soluble
fraction of bio-oil in n-pentane.
Finally, the pH values of bio-oil samples were measured and the
results were given in Table 10. The pH values of bio-oil samples
were found to change between 1.85 and 3.23 which indicates their
acidic characteristic.
It can be concluded from the analysis results given in Tables 2,
710 that after some purifying and improving processes (such as
FischerTropsch synthesis, cracking, hydrogeneration, etc.), bio-oil
samples can be used as an alternative biofuel and chemical
feedstock.
4. Conclusions
The analysis results obtained for the solid products, have
showed that produced biochars can replace the conventional fossil
fuels due to their high xed carbon content and high caloric value.
In addition, the produced biochars can also be used as a carbon
source for producing different carbon materials.
It was found that the bio-oil samples can only be used as an
alternative fuel after application of some purifying and improving
processes. In addition to the analysis performed in this study, it is
necessary to describe important chemical fractions present in bio-
oil samples. These fractions may either be used directly or by
mixing with other conventional fuels.
This experimental work opens encouraging perspectives such as
the evaluation of the biomass residues as a chemical feedstock and
an alternative biofuel. The various thermal degradation processes
such as carbonization, pyrolysis and gasication may help to reduce
deforestation and pollution, while providing greater amounts of
a desirable, renewable fuel and chemical resource.
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Table 10
The pH values of bio-oil samples.
Material pH value
Apricot stone bio-oil 1.85
Hazelnut shell bio-oil 2.95
Grapeseed bio-oil 3.23
Chestnut shell bio-oil 2.63
D. O

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Technical Note

Characterization of biochar and bio-oil samples obtained from carbonization

zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1320

zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1321

zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1322

zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1323

zimen D, Ersoy-Meriboyu A. A study on the carbonization of grapeseed and

zimen D, Ersoy-Meriboyu A. Evaluation of grapeseed as a biofuel source,

zimen D, Ersoy-Meriboyu A, Haykr-Ama H. Effect of temperature on the

zimen, A. Ersoy-Meriboyu / Renewable Energy 35 (2010) 13191324 1324

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