Investigation of thermal behaviour and kinetic
analysis of Pakistani biomass:
Rice husk, sugarcane bagasse and wheat straw
using thermogravimetric analysis
Qari M. K. Waheed1*, Shahid Maqsood2, Rashid Nawaz3, Anas Bin Aqeel4
1
Institute of Mechatronics Engineering, University of Engineering and Technology Peshawar,
Pakistan, 4College of E&ME, National University of Science and Technology, Rawalpindi,
Pakistan, Email: qarikhalid@uetpeshawar.edu.pk
Abstract- Sugarcane bagasse, wheat straw and rice husk
are amongst the most abundantly available agriculture
residues in Pakistan. Constant supply and huge quantities
of these residues make them favourable option to replace
the fossil fuels. Thermal degradation of these three samples
was studied using TGA at three different heating rates of 5
°C min-1, 20 °C min-1 and 40 °C min-1. The three samples
were heated from 25 °C to 900 °C and the influence of
heating rate was investigated. Coats-Redfern method was
applied to calculate the apparent kinetic parameters. The
results showed that the apparent kinetic energy varies
from 28.27 kJ mol-1 to 31.98 kJ mol-1, 38.39 kJ mol-1 to
70.22 kJ mol-1 and 25.05 kJ mol-1 to 30.42 kJ mol-1 for
bagasse, wheat straw and rice husk respectively. A clear
linear fit was obtained using the Coats-Redfern method
with above 0.96 coefficient of regression for wheat straw
and above 0.97 for sugarcane bagasse and wheat straw
respectively. For wheat straw at 40 °C min-1 heating rate
and for the first peak in DTG thermogram of sugarcane
bagasse at 5 °C min-1, the order of reaction was found to be
2.0 and for all three samples, order of reaction was found
to be 0.5 for rest of the heating rates. Higher heating rates
caused the lateral shift in the TGA thermograms of all
three biomass samples but the amount of residual char and
ash were unaffected. It was observed that the higher
heating rate caused the sudden release of volatile matter
from the sample merging the different weight loss peaks, as
were evident at lower heating rate in the DTG thermogram
of sugarcane bagasse. The values of pre-exponential factor
were found to be varied from 12.77-111.08 min-1, 117.92-
1.17x106 min-1 and 21.45 -5.92x104 min-1 for rice husk,
wheat straw and sugarcane bagasse respectively. For order
of reaction of 0.5 at 20 °C min-1 heating rate, three biomass
samples can be arranged in terms of activation energy:
wheat straw > sugarcane bagasse > rice husk.
Keywords— Non-isothermal kinetics, Coats-Redfern
method, Rice husk, Sugarcane bagasse, Wheat Straw,
Kinetic analysis, Biomass kinetics
I. INTRODUCTION
With ever increasing industrial growth, the energy
demand is increasing every year. Biomass has gained an
important position due to its net carbon neutrality. The
amount of carbon dioxide introduced into the atmosphere
978-1-4673-6813-1/15/$31.00 ©2015 IEEE
by thermal decomposition of biomass is taken up by
plants during the process of photosynthesis.
Pakistan has a huge biomass potential, being the fifth
largest sugarcane producer in the world, it is estimated
that 49,373 thousand metric tonnes of sugarcane is
produced annually with the 16,293.09 thousand metric
tonnes of bagasse is available in the form of residue from
sugar industry. Furthermore 1376.6 thousand metric
tonnes of rice husk and 35796 thousand metric tonnes of
wheat straw is available annually from 6883 thousand
metric tonnes of rice and 23,864 thousand metric tonnes
of wheat respectively [1]. These agricultural wastes if not
utilized properly can cause disposal problems in specific
local areas. Owing to the acute power shortage problem,
it is the high time for Pakistan to exploit this vast
potential of biomass. Although the government has
allowed the Pakistan Sugar Mills Association to co-
generate the electricity from bagasse [2] but the process
of conventional combustion is inefficient, leading to
environmental pollution and higher CO2 emission.
Thermochemical processes such as pyrolysis and
gasification are of central importance in recovering
energy from biomass waste. Pyrolysis has gained much
attention as the process can be optimised to obtain the
liquid oils and char while gasification is more favourable
for the production of gaseous products at higher
temperature. Calorific value and density of liquid and oil
products are high which result in higher energy density
as compared to original biomass. In order to design the
efficient thermochemical conversion systems, it is
important to investigate the thermal degradation and
kinetic behaviour of biomass samples.
Thermogravimetric analysis (TGA) is a very popular
technique which is extensively used to investigate the
devolatilization characteristics and kinetic parameters of
different biomass sample. TGA records the weight loss
of biomass sample as a function of temperature. With the
rise in temperature, any loss in sample weight was
recorded by microbalance which holds the sample
containing crucible. It provides a eaningful comparison
of different reaction parameters such as temperature and
heating rate.
Various researchers have studied thermal
degradation behaviour of different biomass materials
under different conditions [3-5]. For example, Ghaly et
al. [4] studied the kinetic parameters of four different
straws (wheat, barley, oats and rye) using TGA. They
reported two reaction zones for all varieties of straw.
For first reaction zone, activation energy and order of
reaction was found in the range of 80-102 kJmol-1 and
1.3-2.3 respectively while for second reaction zone,
activation energy was ranging from 34-75 kJ mol-1 and
the order of reaction was found in the range of 0.1-0.7.
Daood et al. [3] compared the oxidation kinetics of
char from sugarcane bagasse and cotton stalk with
Pakistani coal under 1 % and 3 % oxygen concentration.
Using Coats Redfern method, they found that biomass
char was more reactive than the coal and conversion rate
was increased with the rise in oxygen concentration.
Apparent activation energy for biomass samples was
found to be in the range of 41.2-105.8 kJ mol-1 under 1
% oxygen and 46.9-125.6 kJ mole-1 under 3 % oxygen
concentration. Order of reaction was varying from 0.5 to
2.0. Ataide et al. [5] used sorghum bagasse and tobacco
waste for the investigation of kinetic parameters using
three different methods. They reported activation
energies for tobacco waste, 103.94 kJ mol-1 using
Ozawa method, 135.95 kJ mol-1 using Starink method
and 39.7-272 kJ mol-1 using independent parallel
reaction model. For sorghum bagasse, activation energy
was found to be 120.01 kJ mol-1 by Ozawa method,
148.91 kJ mol-1 for Starink method and 35.7-220 kJ mol-
1
for independent parallel reaction model.
Atimatay et al. [6] investigated the kinetic
parameters of different fresh wood and waste furniture
wood samples using Coats-Redfern method in an air
environment. They reported three regions of weight
loss; first being the moisture weight loss, second region
constitutes the major weight loss from sample, mainly
due to volatiles in the wood sample. Final region was
named oxidation regions as the char left over from
volatiles was oxidised in this region. They reported the
activation energy of 45-136 kJ mol-1 for different
samples of waste wood. It was suggested that the
chemicals used during the processing of treated wood
catalysed the thermal degradation process and hence
lower activation energy was found for treated samples
when compared with the untreated wood samples.
The aim of this study was to investigate the thermal
degradation behaviour of three different biomass
samples from Pakistan and compare their relative kinetic
parameters i.e. order of reaction, activation energy and
pre-exponential factor. Modified Coats-Redfern method
was used to calculate the kinetic parameter. Owing to
the presence of large number of competing parallel
reactions this method was chosen. Also it was assumed
that due to the smaller particle size reaction temperature
is constant within the particle. Another reason for
choosing this method came from the research carried out
by Petrovic et al [7]. They compared the different
methods for determination of kinetic parameters and
concluded the better performance of this method over
the others.
II. MATERIALS AND METHODS
A. Materials
Sugar cane (saccharum officinarum) bagasse, Rice
(Oryza sativa) husk and wheat (Triticum aestivum)
straw samples were sourced from Pakistan. Being the
agricultural nation, wheat is one of the major crops of
the country. Due to the better incentives from
government in terms of price, only in 2011-2012 fiscal
year Pakistan produced more than 24 million tonnes of
wheat [8]. Wheat straw samples were collected from
known fields near Faisalabad city (31 21 N, 72 59 E).
Only Punjab province accounts for almost two third
of the total sugarcane (saccharum officinarum)
production [9]. Plantation can be done either in spring or
autumn. Most of the plantation in Punjab province is
done in spring with the growth period of 8-10 months.
This sample was obtained from spring plantation with
the growth period of 9 months. Sugarcane samples were
obtained from known field near Samundri (30 48 N 71
52 E). These fields provide sugarcane to Gojra
Samundri Sugar Mills Limited.
Rice (Oryza sativa) is also one of the most important
crops in Pakistan. The country is famous for the
production of its world’s finest long grained basmati
rice also known as basmati Pak-10. During last year,
Pakistan showed a 28% rise in rice production totaling
up to 6.16 million tonnes [10]. Rice husk samples were
obtained from known fields in Faisalabad city (31 21 N,
72 59 E).
When received, samples were bagged in plastic bags.
Samples were grinded and sieved to the 1.4-2.8 mm
particle size and kept in air tight containers to ensure the
consistent composition until final usage. Before kinetic
study, proximate and ultimate analysis of the samples
was performed and results are shown in Table I.
B. Thermogravimetric Analysis
 A Stanton Redcroft 1000 TGA operating at Where A is pre-exponential factor (min-1); E is
atmospheric pressure was used to carry out the apparent activation energy (kJ mol-1); T is reaction
thermogravimetric analysis of the biomass samples. temperature (K); R is gas constant which is equal to
Thermoquest CE instrument flash EA 1112 series was 8.314  10-3 (kJ mol-1 K-1).
employed for C, H, N and S analysis of the biomass
After incorporating non-isothermal heating rate β =
samples. During thermogravimetric analysis, 15 mg of
each biomass sample was heated from room temperature dT/dt and the value of reaction rate constant k from
to 900 °C with a dwell time of 10 min. All the “(3)” in “(1)”.
experiments were performed using nitrogen as a carrier
dα A E
gas. Each sample was analyzed at three different heating  f (α ) exp(
) (4)
rates of 5, 20 and 40 °C min-1. The weight loss of each dT β RT
biomass sample with time and with the rise in As f(α) = (1-α)n incorporated in “(4)” and solving for
temperature was continuously recorded. This raw data the exponential term, “(4)” becomes
was used to draw thermogravimetric (TG) and  dα  A E
differential thermogravimetric (DTG) thermograms. ln  dT  ln[ ].(
) (5)
 (1
α ) n β RT
C. Calculation of Kinetic Parameters 

A detailed description of processing non-isothermal

kinetic data by using a modified Coats-Redfern method Proximate Analysis (ash-free basis)
has been reported and discussed in [11]. Volatile Fixed Moistur
Feedstock
matter carbon e
The basic kinetic equation is written in “(1)” as
(wt.%) (wt.%) (wt.%)
shown below.
Bagasse 82.89 11.09 6.02
dα
 kf (α ) (1) Rice husk 76.95 15.68 7.37
dt
Wheat Straw 78.41 18.76 2.82
Where α is the conversion of the biomass, defined
as in “(2)”. Ultimate analysis
Feedstock
m
m C H N O*
α 0 (2)
m0
m (wt.%) (wt.%) (wt.%) (wt.%)

Bagasse 45.5 5.63 0.8 48.07

Where m0 is the initial sample weight, m is the
Rice husk 39.82 5.4 1.27 53.51
sample weight at time t , and m is the final sample
Wheat Straw 32.96 4.33 1.18 61.53
weight. The reaction rate constant, k is given by the TABLE I. PROXIMATE AND ULTIMATE ANALYSIS OF
FEEDSTOCK

A plot of LHS of “(5)” against 1/T corresponds to a

straight line exhibiting a slope of –E/R for different
values of n with a coefficient of regression (R2) close to
unity. For each biomass sample, the values of E and A
are calculated for four different value of reaction order
n, (0.5, 1.0, 1.5 and 2.0) for each weight loss curve in
TGA thermogram for each heating rate. The order of
reaction with the coefficient of regression closest to
unity was reported as a final result.

III. RESULTS AND DISCUSSION

From the proximate analysis results shown in Table
Arrhenius equation as in “(3)”. I, it can be indicated that relatively higher volatiles were
present in bagasse and wheat straw samples. The highest
E
k  A exp(
) (3) volatiles in bagasse, presented on ash-free basis,
RT accounted for around 83% of the total weight. 78.41
wt.% of volatiles were found in wheat straw sample
while slightly lesser 76.95 wt.% were present in rice
husk. The amount of fixed carbon in wheat straw was
18.76 wt.%. For rice husk and bagasse it was found to
be 15.68 wt.% and 11.09 wt.% respectively.
Relatively higher ash contents were found in rice
husk sample. The amount of residual ash found was 1.62
wt.% for bagasse, 6.9 wt.% for wheat straw and 17.21
wt.% for rice husk. Higher ash contents in rice husk
were also reported by other authors [12]. In-depth
investigation results of chemical composition of ash
from 86 different biomass samples were collected and
presented by Vassilev et al. [13]. They reported that ash
from rice husk contains 94.48 wt.% of SiO2 as compared
to 46.79 wt.% for bagasse and 50.35 wt.% for wheat
straw. Other species found in ash were CaO, MgO, K2O,
P2O5, Al2O3, Fe2O3 and Na2O.
A. The Influence of Heating Rate
The influence of heating rate on the devolatilization
behaviour of rice husk, bagasse and wheat straw was
investigated using TGA. Three different heating rates of
5, 20 and 40 °C min-1 were employed during this
investigation. TGA and DTG thermograms of rice husk,
bagasse and wheat straw were shown in Fig.1, Fig. 2 and
Fig. 3 respectively. It has been reported by several
authors [14, 15] that the higher heating rates caused the
lateral shift in the TGA thermograms of sugarcane
bagasse sample but the amount of residual char and ash
were unaffected by the heating rate. Similar trends were
observed for the wheat straw and rice husk biomass
samples however with the increase in heating rate, an
increase in residual char contents was reported in [16,
17].
Fig. 1. TGA and DTG thermograms of rice husk at 5, 20 and 40°C
min-1 heating rates
Fig. 2. TGA and DTG thermograms of sugarcane bagasse at 5, 20
and 40°C min-1 heating rates
The effect of heating rate on TGA and DTG
thermograms of rice husk was shown in Fig. 1. From the
TGA thermogram it is clear that the increase in heating
rate shifted the release of volatiles to the slightly higher
temperature. It was suggested in the literature [16, 18]
that this lateral shift was primarily due to the heat
transfer limitations at higher heating rates. Due to short
reaction time at higher heating rates, higher temperature
was required for the evolution of volatiles from biomass
samples while at slow heating rates, large instantaneous
energy along with longer residence time was available
for the volatiles to evolve from biomass. Williams et al.
[14] examined the weight loss behaviour of rice husk
and its individual components such as cellulose,
hemicelluloses and lignin. With the increase in heating
rate, they also reported a shift in TGA thermogram
towards higher temperature. DTG thermogram showed
initial weight loss attributed to the moisture loss while
the major weight loss observed between 250 °C to
450 °C was due to the thermal decomposition and
release of volatiles from rice husk.
TGA and DTG thermograms of sugarcane bagasse
sample shown in Fig.2 represent the influence of heating
rate. It is observed in DTG thermogram that at 5 °C min-
1
heating rate, a small weight loss peak was observed
around 300 °C before the main weight loss peak. This
effect is more pronounced at 20 °C min-1 heating rate.
Further increase in heating rate to 40 °C min-1 caused
the two peaks to merge together. Similar behaviour was
reported in [19]. This gradual weight loss behaviour at
lower heating rates which was not evident in the DTG
thermograms of rice husk and wheat straw, can be
correlated to the variation in amount of cellulose and
hemicellulose contents in the sugarcane sample. As
reported previously, the smaller peak around 300 °C can
be correlated to the decomposition of hemicellulose
present in bagasse and major weight loss peak was
attributed to the decomposition of cellulose. It is
suggested that the later shift caused by the increase in
heating rate merged the two peaks. Similar behaviour
was also reported by Slopiecka et al. [18]. However with
the increase in temperature, opposite trend of separation
of different peaks was reported in [15]. TGA and DTG
thermograms of wheat straw shown in Fig.3 showed
similar behaviour to rice husk.
Fig. 3. TGA and DTG thermograms of wheat straw at 5, 20 and
40°C min-1 heating rate
coefficient of regression of > 0.97. For wheat straw, it
was found to be from 38.39 kJ mol-1 to 70.22 kJ mol-1.
For bagasse energy of activation was from 28.27 kJ mol-
1
to 31.98 kJ mol-1. The coefficient of regression was >
0.96 and > 0.97 for wheat straw and sugarcane bagasse
respectively.

B. Kinetic Parameters The order of reaction of 0.5 was established at all

Pyrolysis of biomass is a complex process heating rates for rice husk. For wheat straw also order of
comprising of various competing parallel and series reaction was found to be 0.5 for 5 °C min-1 and 20 °C
reactions. The use of TGA data to calculate kinetic min-1 but at 40 °C min-1 heating rate, order of reaction
parameters including activation energy, pre-exponential was found to be 2.0. For sugarcane bagasse, small
factor and order of reaction provides the general shoulder aroused at 5 °C min-1 heating rate showed the
information about the overall reaction kinetics rather order of reaction of 2.0 while the main peak at 5 °C min-
1
than individual reactions. However these kinetic showed the order of reaction of 0.5. Other higher
parameters calculated from the TGA data are useful heating rates also showed the 0.5 order of reaction for
when comparing the reaction parameters such as sugarcane bagasse.
reaction temperature and heating rates. Activation
The value of pre-exponential factor was found to be
energy varies reaction rate with respect to temperature
varied from 12.77-111.08 min-1, 117.92-1.17x106 min-1
while pre-exponential factor is related to the material
and 21.45 -5.92x104 min-1 for rice husk, wheat straw and
structure.
sugarcane bagasse respectively.
Non-isothermal technique is simple and better way
Mansaray et al. [21] studied the different varieties of
of finding the kinetic parameters of biomass samples. In
rice husk sample to calculate the kinetic parameters.
this study, Coats-Redfern method was used to calculate
They used 99.5 % oxygen as a medium for reaction.
the kinetic parameters using non-isothermal kinetic data
They find the values of 142.7- 188.5 kJ mol-1 for the
from TGA. A detailed description of processing non-
main decomposition zone.
isothermal kinetic data by using a modified Coats-
Redfern method has been reported and discussed in [11]. TABLE II. RESULTS FROM COATS-REDFERN METHOD.
Procedure to calculate the kinetic parameter from raw
data using Coats-Redfern method was outline in [20]. Heating rate 5 °C min-1
Three different heating rates were employed to obtain
Feedstock Temp Ea A R2 n
the consistent and more reliable results. As mentioned in
the previous section, three distinct reaction zones were (°C) (kJ/mol) (min-1)
observed during the thermogravimetric analysis. Major Rice husk 230-360 27.96 12.77 0.982 0.5
weight loss was observed during the second zone around Wheat
400 °C. At lower heating rate of 5 °C min-1, sugar cane straw 230-330 38.39 177.92 0.974 0.5
bagasse sample showed a clearly separate weight loss Bagasse 190-230 28.68 21.45 0.993 2.0
peak separating from the main peak (Fig. 2). Hence two
Bagasse 240-360 28.27 59247.25 0.974 0.5
set of kinetic parameters were calculated for sugarcane
-1
Heating rate 20 °C min
bagasse at 5 °C min-1 heating rate. At higher heating
rates, only one set of kinetic parameters was calculated Rice husk 220-390 25.05 19.59 0.972 0.5
because both peaks merged and appeared as one. For Wheat
straw 230-350 38.42 433.91 0.968 0.5
rice husk and wheat straw samples only one set of
kinetic parameters were calculated at each heating rate Bagasse 200-380 29.89 56.56 0.988 0.5
as shown in Table II. Heating rate 40 °C min -1

Final results from Coats-Redfern method are shown Rice husk 240-430 30.42 111.08 0.976 0.5
in Table II. For a single reaction, activation energy is a Wheat
straw 260-430 70.22 1170293 0.961 2.0
single constant value but biomass thermal degradation is
a complex process with several competing reactions. Bagasse 200-450 31.98 145.02 0.988 0.5
The activation energy reported here is global activation Comparison of Activation energy from Literature
energy or apparent activation energy of the entire Numerous studies [19, 21-27] have attempted to
process. The activation energy of rice husk was found to explain the kinetic parameter from TGA data but there is
be varied from 25.05 kJ mol-1 to 30.42 kJ mol-1 with the a wide variation in kinetic parameters values. These
variations are mainly due to the type of method applied The influence of heating rate was also investigated
to calculate the kinetic parameters, heating rate, type of on all three biomass samples. It was indicated that the
biomass and whether the experiment was carried out in increase in heating rates caused the lateral shift in the
inert atmosphere or in oxygen atmosphere. A TGA thermograms. It is suggested that this behaviour
comparison of activation energy values of the current was due to short reaction time at higher heating rates,
study to that of literature is outlined in Table III. that’s why higher temperature was required for the
TABLE III. COMPARISON OF ACTIVATION ENERGY OF
evolution of volatiles from biomass samples.
BIOMASS SAMPLES
Kinetic parameters including activation energy, pre-
exponential factor and order of reaction were calculated
Activation Energy (kJ mol- using Coats-Redfern method. For rice husk, order of
1
) ref
Feedstock
reaction was found to be 0.5 for all heating rates. For
During During wheat straw it was 0.5 for 5 °C min-1 and 20 °C min-1
Pyrolysis Combustion
but for 40 °C min-1 heating rate, order of reaction was
This changed to 2.0. For bagasse, first peak exhibited 2nd
Rice Husk 25.05 - 30.42 - study
order while 0.5 order of reaction was calculated for
This
Wheat Straw 38.39 - 70.22 - study
second peak. In addition to that, activation energy
This results were compared with the various other biomasses
Bagasse 28.27 - 31.98 - study in literature.
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