Journal of Analytical and Applied Pyrolysis 121 (2016) 403–408

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Journal of Analytical and Applied Pyrolysis

journal homepage: www.elsevier.com/locate/jaap

Thermo-chemical conversion of mango seed kernel and shell to value

added products
Gautam Ganeshan 1 , Krushna Prasad Shadangi 2 , Kaustubha Mohanty ∗
Department of Chemical Engineering Indian Institute of Technology Guwahati, Guwahati, 781 039, India

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

Article history: Mango (Mangifera indica) is one of the popular fruits in India and many other tropical countries also.
Received 28 June 2016 Mango seed weight is 30 − 45% of the total fruit weight which completely goes off as waste. In this
Accepted 3 September 2016 study, Mango seed kernel (MSK) and Mango seed shell (MSS) were selected as a feed for pyrolysis for the
Available online 4 September 2016
production of bio-chemicals. Conventional pyrolysis of MSK and MSS was carried out in the range between
673 to 873 K temperatures at a heating rate of 25 K min−1 . The optimum temperature for maximum yield
Keywords:
of pyrolytic liquid was 823 K and 848 K for MSK and MSS with the corresponding yield of pyrolytic liquid
Mango seed
of about 32.37% and 52.57% respectively. The composition analysis of MSK and MSS pyrolytic liquid
Mango shell
Pyrolysis
revealed the presence of various valuable chemicals. It was noticed that MSS pyrolytic liquid contains
Pyrolytic liquid about 27.63% d-allose, which is a rare sugar, whereas MSK contains 13.27% of levoglucosan along with
Rare sugar furfural, furan, alcohol, aldehyde, benzene and various alkanes.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction
Mango (Mangifera indica) is most popular fruit grown in tropi-
cal and subtropical countries and is one of the most common edible
fruit all over the world. Mango and mango products such as pick-
les, nectar, chutney, canned pulp and slices have gained worldwide
popularity. The waste products from this fruit (i.e., mango peel and
seed) have not been put to any serious use till date. Mango seed
which accounts for 30 − 45% of the total fruit weight depending
on its variety is the major waste product from mango process-
ing industry [1]. In India, mango is known as the “king of fruits”
and India itself accounts for 15.03 million tons of mango produc-
tion which contributes to 40.48% of the world mango production.
Total mango production of the world in 2010 was around 37.12
million tons [1,2]. The weight of Mango seed accounts for more
than 30% of the total fruit weight. The fat content is around 10%
of the weight of the seed. The fatty acid composition (oleate and
stearate) of matured mango seed varies with its variety [3]. Ali
et al. and Abdalla et al. reported that the extraction of lipids was
possible using methanol as solvent in solvent extraction process
∗ Corresponding author.
E-mail address: kmohanty@iitg.ernet.in (K. Mohanty).
1
Present address: Department of Chemical Engineering, C.V. Raman Institute of
Technology, Bhubaneswar, Odisha, India.
2
Present address: Department of Chemical Engineering, V. S. S. University of
Technology, Burla, Odisha -781018, India.
from different variety of mango seed kernel [4,5]. Along with these
extractives, hemicelluloses, cellulose and lignin are the other con-
stituents of mango seed kernel and shell. Upon thermal treatment,
these offer various chemicals along with char. Literatures reveal
pyrolysis of seeds can be a sources various valuable bio-chemicals
[6–15]. Cellulose is a remarkable pure organic polymer, consisting
solely of units of anhydro-glucose held together in a giant straight-
chain molecule. These anhydro-glucose units are bound together by
␤-(1,4)-glycosidic linkages [16]. The degradation reaction of cel-
lulose is characterized by the decrease in polymerization degree.
Thermal degradation of cellulose can either proceed through grad-
ual degradation, decomposition and charring on heating at lower
temperatures or through rapid volatilization accompanied by the
formation of levoglucosan during pyrolysis at higher temperatures.
The glucose chains in cellulose are first cleaved to glucose and from
this, during second stage, glucosan is formed by the splitting of one
molecule of water [16]. Hemicelluloses are derived mainly from
chains of pentose sugars, and act as the binding material holding
together the cellulose units and fibre. Hemicellulose decomposes
readily forming furan and furan derivatives. Lignins are polymers
of aromatic compounds. It is a macro-molecule, which consists
of alkyl-phenols and has a complex three-dimensional structure.
Pyrolysis of lignin yields more than 51% of phenol and methyl phe-
nol derivatives which constitute the dark oil [17]. The extractives
content in biomass also plays a significant role in the product dis-
tribution of biomass pyrolysis. Lignin and extractive content of the
biomass determine the possibility of formation of the tarry liquid. If

http://dx.doi.org/10.1016/j.jaap.2016.09.004
0165-2370/© 2016 Elsevier B.V. All rights reserved.
404 G. Ganeshan et al. / Journal of Analytical and Applied Pyrolysis 121 (2016) 403–408
the lignin or extractive content of the biomass is less, the pyrolysis
product results in lesser amount of tarry liquid and so it may be
considered for extraction of valuable chemicals instead [18].
The present study reports the best use of one of the agricultural
waste such as mango seed kernel (MSK) and mango seed shell (MSS)
for the production of various valuable chemicals using pyrolysis
technique.
2. Materials and methods
2.1. Preparation of raw materials
Mango seeds were collected from the fruit juice stall of IIT Guwa-
hati, Assam, India. The seeds were properly washed in tap water to
remove the remaining fruit pulp. Then the seeds were sun dried for
48 h followed by oven drying for another 24 h at about 333 ± 5 K.
The seed kernel was separated from the seed shell manually with
the help of knife and both the kernel and shell were grinded to pow-
der by using a mixer grinder (Bajaj, India). The mango seed kernel
(MSK) and mango seed shell (MSS) were passed through sieve and
a particle size of 75 ␮m (ASTM 200 mesh) were collected and stored
in air-tight polythene bags for further use.
2.2. Characterization of MSK and MSS
2.2.1. Proximate and ultimate analysis
Proximate analysis of MSK and MSS was carried out using
standard methods reported elsewhere [6–9], whereas, Eurovector
EA3000 (CHNS) elemental analyzer determined the amount of C,
H, N (ultimate analysis). The high heating value (HHV) was deter-
mined using the formula given by Demirbas [9].
HHV = {33.5[C] + 142.3[H] − 15.4[O] − 14.5[N]} × 10−2 MJ kg−1
(1)
2.2.2. Fourier transform infrared spectroscopy (FTIR) analysis
The FTIR analysis of the MSK and MSS were carried out
using Excalibur Bio-Rad spectrophotometer (model FTS 3500 GX)
attached with DRS (Diffuse Reflectance Spectroscopy). Prior to FTIR
analysis, KBr was oven dried at 333 K for 1 h and powdered by using
mortar pestle. The powdered KBr was mixed with samples (1:100)
and placed in the sample holder and the IR spectra were collected
at scan rate of 40 with a step size of 4 cm−1 within the range of 400
to 4000 cm−1 .
2.2.3. EDX analysis
Finely powdered MSK and MSS were analyzed to identify the
presence of various minerals which varies according to the soil
characteristics of the place of growth of Mango tree. The min-
eral content of MSK and MSS were determined using LEO 1430 VP
SEM/EDX analyzer.
2.3. Pyrolysis of MSK and MSS
Pyrolysis of MSK and MSS were carried out in the temperature
range between 673 and 873 K, at a heating rate of 25 K min−1 using
a semi-batch reactor made up of stainless steel (Length: 21 cm, ID:
6 cm). The reactor was filled with 40 g of feed samples and heated
by a self-fabricated electrical heated cylindrical furnace where the
set temperature was maintained by a PID controller. The generated
volatiles were condensed by a water cooled glass condenser. The
liquid product was collected in a measuring cylinder and weighed.
At the end of the process, the reactor was cooled and the remaining
char was collected from the reactor and weighed. The weight% yield
of pyrolytic liquid, char, gas and conversion of feed to products were
calculated using Eqs. (6)–(9).
%Liquid yield = (Liquid weight/Feed weight) × 100 (6)
%Char yield = (Char weight/Feed weight) × 100 (7)
%Gas yield = 100-(%Liquid yield + % Char yield) (8)
%Conversion = (wt. of raw material-wt. of char)/wt. of
raw material (9)
2.4. Characterization of MSK and MSS pyrolytic liquid
2.4.1. FTIR analysis
The functional groups present in MSK and MSS pyrolytic liquid
were determined using DRS attached Excalibur Bio-Rad spec-
trophotometer (model FTS 3500 GX) FTIR analyzer within the range
of 400–4000 cm−1 at scan rate of 40 with a step size of 4 cm−1 . One
drop of liquid sample was added to KBr pellet and the IR spectra
were collected and analyzed.
2.4.2. GC–MS analysis
The composition of MSK and MSS pyrolytic liquid obtained at the
optimum temperature were determined and discussed. The GC–MS
analysis was performed using Perkin Elmer Clarus680 GC/600C
MS analyzer. The GC was programmed at 313 K for 0.5 min with
the total run time of 30 min. The temperature was increased at
the rate of 10 K min−1 to 573 K. Elite 5 MS column of diameter
0.250 ␮m, length 30 m was used. Exact 1 ␮L volume of sample was
injected into the column with a carrier gas (Helium) flow rate of
0.6 mL min−1 .
3. Results and discussion
3.1. Physical properties of MSK and MSS
The physical properties of MSK and MSS are discussed from the
outcomes of proximate, ultimate and EDX analysis. The proximate
and ultimate analysis is displayed in Table 1. From the analysis,
it was observed that the 48 h sundried and 24 h oven dried MSK
and MSS hold 11% and 10.42% of moisture respectively. Both MSK
and MSS were rich in volatile matters followed by fixed carbon
and ash content. Volatile matters are responsible for the forma-
tion of gaseous products such as carbon monoxide, carbon dioxide,
methane, free nitrogen etc. along with condensable volatiles during
thermochemical conversion (pyrolysis). Fixed carbon is the com-
bustible residue left after the expulsion of volatiles. Fixed carbon
along with the ash constitutes the char that formed during pyrol-
ysis. More amount of fixed carbon in the biomass yield a higher
amount of char during pyrolysis. Proximate analysis confirmed that
MSK was rich in fixed carbon compared to MSS, thus, more amounts
of char may be expected out of MSK pyrolysis. Ash is that part of
a material which doesn’t burn. The amount of ash in both MSK
and MSS was very less therefore making them a suitable feed for
pyrolysis to produce more liquid products.
Table 2 shows the various minerals present in MSK and MSS
determined by EDX analysis. It was noticed that MSK was compara-
tively less rich in minerals whereas, MSS contains various minerals.
Among all, magnesium was higher in MSS followed by Fe, Co, Ni,
Cu and Zn, which can be extracted using various techniques as
value added products. The presence of such minerals act as catalysts
during pyrolysis to enhance the rate of various reactions [19].
FTIR analysis characterized the raw materials as shown in Fig. 1.
The IR peaks observed in the range of 3200–3400 cm−1 indicated
the presence of moisture in the sample which could be due to the
 G. Ganeshan et al. / Journal of Analytical and Applied Pyrolysis 121 (2016) 403–408 405

Table 1
Physical properties of MSK and MSS.

Proximate analysis

Sample Moisture (%) Volatile Matter (%) Ash (%) Fixed Carbon (%)
MSK 11.08 67.23 1.10 20.59
MSS 10.42 71.69 0.58 17.02

Ultimate analysis
Sample N (%) C (%) H (%) O (%) Calorific Value (MJ kg−1 )
MSK 0.212 43.629 6.374 49.785 15.988
MSS 0.255 45.832 1.093 52.820 8.737

Table 2 50
Minerals composition of MSK and MSS by EDX analysis. (a) Pyrolytic char
Pyrolytic liquid
Minerals MSK (%) MSS (%) Non-condensable gas
45
Al 1.37 0.06
Mn – 19.34
Fe – 10.43 40
Co 2.21 8.28
Ni – 4.16

% Yield
Cu 0.58 2.52 35
Zn – 1.67
As – 0.28
Si 3.08 – 30
K 0.54 –

25

90 MSK
MSS 20
650 700 750 800 850 900
80
Temperature (K)
70

60 235 7 1444
60
2845
%T

Pyrolytic cha r
50 (b) Pyrolytic liquid
55 Non-cond ensab le gas
40
2139 1529 50
30
145 6 45
20
% Yield

2906 40
1629
3356
10
450 0 400 0 350 0 300 0 250 0 200 0 150 0 100 0 500 35
Wave nu mbers, cm -1 30
Fig. 1. FTIR spectra of MSK and MSS.
25

axial deformation of O H group. The presence of carbonyl group 20

(C H groups) ascertained the presence of hemicelluloses which
was confirmed by the peaks in between 2850 and 3000 cm−1 . The
symmetric deformation of CH2 denoted the presence of celluloses
and C C aromatic stretching vibration signified the occurrence
of lignin that was oobserved in between 1400 and 1500 cm−1
and1500–1700 cm−1 respectively [9].
3.2. Effect of temperature on pyrolytic yield
The effect of temperature on pyrolytic yield from MSK and MSS
pyrolysis is shown in Fig. 2(a, b). It was observed that the yield of liq-
uid increased up to 823 K for MSK and 848 K for MSS and decreased
with further increase in temperature. The corresponding yield of
pyrolytic liquid was 32.37% and 52.57% for MSK and MSS respec-
tively. Further increase in temperature enhanced the formation of
non-condensable gases and reduced the formation of char. High
temperature pyrolysis results in lighter gaseous products such as
650 700 750 800 850 900
Temperature (K)
Fig. 2. Effect of temperature on pyrolytic yield (a) MSK and (b) MSS.
H2 , CO and CH4 due to secondary cracking of primary pyrolytic
vapors as well as lignin compounds [6–8]. The effect of tempera-
ture on conversion is shown in Fig. 3. The high temperature boosts
the conversion of char to form volatiles and thus, the conversion
in addition to the formation of non-condensable gases increased
[10–16].
3.3. FTIR analysis of pyrolytic liquids
The FTIR analysis of MSK and MSS pyrolytic liquids obtained at
the optimum temperature were analyzed and shown in Fig. 4(a,
b). The detailed descriptions on the functional groups obtained
406 G. Ganeshan et al. / Journal of Analytical and Applied Pyrolysis 121 (2016) 403–408

80 Table 3
MSK FTIR analysis of MSS and MSK pyrolytic liquid.
MSS
Wave numbers, Assignments Compounds
cm−1
75
% Conversion of feed

3200–3570 O H stretching H, bonded hydroxyl group

2800–3050 C H stretching Alkanes
1640–1780 C O stretching Ketones, Aldehydes, Carboxylic acids
1490–1550 NO2 Stretching Nitrogenous compounds
70 1450–1510 C C C stretching Aromatic compounds
1350–1465 C H stretching Alkanes
1260–1350 O H in a plane Primary or secondary alcohol
stretching
65 1150–1250 C O Stretching Phenol
1000–1100 O H stretching Primary alcohol
650–900 O H stretching Phenols, Ethers, Esters, Aromatics

60
650 700 750 800 850 900
Table 4
Temperature (K) Compounds identified by GC–MS of MSK pyrolytic liquid.

Fig. 3. Effect of temperature on conversion of feed. Retention time, min Compound name Area%

8.35 Butanoic acid 2.178

8.54 Methyl propionate 0.720
200 9.12 1-Penten-3-one 0.667
(a) 9.86 Furfural 1.788
180 9.93 2-Cyclopenten-1-one 2.892
10.14 3-Furanmethanol 10.214
160 11.38 Ethanone, 1-(2-furanyl)- 2.388
11.45 Butocarboxim 2.316
140
11.88 Furan, 2-methoxy- 0.291
120 12.02 1,2-Ethanediol, dipropanoate 0.639
12.07 Ethane-1,1-diol dipropanoate 0.391
100 12.37 2-Furancarboxaldehyde, 5-methyl- 0.502
%T

12.51 Silacyclohexadiene-2,5 3.569

80 13.03 3-Heptene, 2-methyl-, (E)- 0.751
1057
1394 13.58 2-Ethyl-5-propylcyclopentanone 2.077
60 13.84 2-Cyclopenten-1-one, 2,3-dimethyl- 0.372
1278 13.95 Phenol, 2-methyl- 0.666
40
14.28 Phenol, 3-methyl- 0.709
20 15.20 4,5-Diamino-2-hydroxypyrimidine 2.600
1640
16.93 1,4:3,6-Dianhydro-.alpha.-d-glucopyranose 4.587
0 17.24 Cyclopentanecarboxamide, n-methallyl- 0.513
3380
17.45 Hydroquinone 4.103
-20 18.59 1,3-Benzenediol, 2-methyl- 0.763
4500 4000 3500 3000 2500 2000 1500 1000 500 21.06 Levoglucosan 13.269
-1
Wave numbers, cm

from MSK and MSS pyrolytic liquids are reported in Table 3. It was
350 observed that both MSK and MSS pyrolytic liquids had similar func-
(b) tional groups. It can thus predicted the possibility of existence of
300 similar bio-chemicals in MSK and MSS pyrolytic liquid.

250 3.4. Gas chromatography–mass spectrometry (GC–MS) analysis

The GC–MS analysis of MSK and MSS pyrolytic liquid at optimum

200 temperature was studied and given in Tables 4 and 5. This analysis
confirmed that both MSK and MSS pyrolytic liquids were mixture
%T

150 of several chemical compounds. Both these pyrolytic liquids consist

of acids, alcohols, esters, phenols, sugars, aldehydes and aromatic
100 compounds, however with dissimilar proportions. MSS pyrolytic
liquid contains higher area% of furfural, furan, aldehyde, ketone,
benzene and various alkane compounds compared to MSK pyrolytic
50 liquid. The major compounds such as D-allose and levoglucosan
1280 were detected by 27.63 area% and 13.27 area% from MSS and MSK
1384
0 1713 pyrolytic liquids respectively. D-allose (C6 H12 O6 ) is a novel and rare
1647 1045
sugar which enhances anti-tumor effect which causes cancer cell
4500 4000 3500 3000 2500 2000 1500 1000 500 growth inhibition, by inducing the tumor suppressor gene thiore-
doxin interacting protein (TXNIP) [20]. Levoglucosan (C6 H10 O5 ) is
-1
Wave numbers, cm an organic compound having six carbon ring structure formed by
the pyrolysis of carbohydrates, such as starch and cellulose. The
Fig. 4. FTIR spectra of (a) MSK pyrolysis liquid and (b) MSS pyrolysis liquid. hydrolysis of levoglucosan can produce fermentable sugar glucose
 G. Ganeshan et al. / Journal of Analytical and Applied Pyrolysis 121 (2016) 403–408 407

Table 5 matic in nature and its pyrolysis leads to formation of phenolic

Compounds identified by GC–MS of MSS pyrolytic liquid.
aromatic compounds. Most of the aromatic compounds found in the
Retention time, min Compound name Area% pyrolytic liquids are result of decomposition of lignin. The degra-
8.34 Methyl-.beta.-l-arabinopyranoside 0.997 dation of carbohydrates leads to the formation of 3-furanmethanol
8.54 Heptane, 1,1 -oxybis- 1.692 and other such compounds [23].
8.75 Etilefrin-propionyl 1.023
9.13 1-Penten-3-one 0.408
9.87 Furfural 4.639 4. Conclusions
9.94 3-(4,8,12-Trimethyltridecyl) furan 0.964
10.21 1,1-Dimethyl-1-silacyclobutane 0.858 From this study, it was concluded that pyrolysis technique
10.99 Furan, tetrahydro-2,5-dimethoxy- 0.409
11.35 2-Cyclopenten-1-one, 2-methyl- 0.480
can be used to produce various valuable chemicals from waste
11.39 Bicyclo[3.2.0]Heptan-2-one 1.269 biomass. MSS and MSK are such wastes which have negligible use
12.03 1,2-Ethanediol, Dipropanoate 0.455 in our daily life and were almost thrown away. However, it was
12.38 2-Furancarboxaldehyde, 5-methyl- 1.096 very clear that such waste materials can be a raw material for
12.52 Silacyclohexadiene-2,5 0.693
the production of D-allose (which is an epimer of Glucose and a
13.04 6,7-Dimethyl-9-oxo-1,5- 1.924
diazabicyclo[5.2.0]non-5-ene very rare sugar), Levoglucosan and 3-Furanmethanol along with
13.58 2-Ethyl-5-propylcyclopentanone 1.924 various bio-chemicals. This result also confirmed that MSS was
13.95 Phenol, 2-methyl- 0.843 suitable for D-allose production and MSK for Levoglucosan and 3-
14.75 Phenol, 2-methoxy- 1.805 Furanmethanol production. It was observed that the D-allose and
14.98 Heptane, 1,1 -oxybis- 1.311
levoglucosan were found to be 27.63 area% and 13.27 area% from
15.20 Maltol 0.874
15.61 Phenol, 2,4-dimethyl- 0.511 MSS and MSK pyrolytic liquids respectively. Apart from these, about
16.44 Phenol, 2-methoxy-4-methyl- 3.353 10.21 area% of 3-Furanmethanol was present in MSK pyrolytic oil
16.80 2-Furancarboxaldehyde, 5-(hydroxymethyl)- 1.005 whereas MSS pyrolytic oil included 11.16 area% of Phenol and 4.64%
16.93 1,4:3,6-Dianhydro-.alpha.-d-Glucopyranose 1.405
of Furfural. Currently, more emphasis has to be given for the purifi-
17.25 Cyclopentanecarboxamide, n-methallyl- 0.702
17.45 Pentanoic acid, 2-ethylcyclohexyl ester 0.990 cation of such pyrolytic liquid, which is the future prospective of
17.63 1,2-Benzenediol, 3-methoxy- 0.566 this study.
17.75 Phenol, 4-ethyl-2-methoxy- 0.752
18.03 (Z)-4-Methyl-5-(2-oxopropylidene)-5h-furan- 0.985
2-one Acknowledgements
18.75 Phenol, 2,6-dimethoxy- 2.775
19.64 Vanillin 0.622 Authors acknowledge the analytical facilities at the Central
20.02 1,2,4-Trimethoxybenzene 2.084
20.22 Phenol, 2-methoxy-4-(1-propenyl)-, (E)- 0.532
Instrumental Facility (CIF), IIT Guwahati as well as the analytical
20.77 Ethanone, 1-(4-hydroxy-3-methoxyphenyl)- 0.472 laboratory at Department of Chemical Engineering, IIT Guwahati.
21.18 D-Allose 27.63
21.52 Hept-5-one-1-lic acid, 4,4-dimethyl-, ethyl 1.733
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