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Experimental Analysis of Tamarind Seed Powder-Based Ash Powder Composition For Eco-Friendly Firecrackers
Experimental Analysis of Tamarind Seed Powder-Based Ash Powder Composition For Eco-Friendly Firecrackers
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Manikandan Rajendran,
Rajajeyaganthan Ramanathan,
P. Ganesan & Rajesh Shanmugavel
ISSN 1388-6150
Volume 143
Number 4
1 23
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Journal of Thermal Analysis and Calorimetry (2021) 143:3009–3021
https://doi.org/10.1007/s10973-020-09707-7
Received: 17 November 2018 / Accepted: 13 April 2020 / Published online: 29 April 2020
© Akadémiai Kiadó, Budapest, Hungary 2020
Abstract
In this work, considering the various practical concerns during storage, processing, handling and emission of flash powder
used for making firecracker, a slight modification was made in chemical composition of flash powder to overcome all the
above-mentioned practical concerns. Generally, flash powder chemical composition consists of K NO3-60%, Al-20% and
S-20% for making firecrackers. The modification was made by replacing 5% and 10% of sulfur with tamarind seed powder
(TSP) in the flash powder composition. In this study, all the chemicals used for making flash powder were of nanometer
size. Using this TSP-based flash powder, the bijili crackers were fabricated and tested for noise level. The performance of
the noise level by TSP-based flash powder was within the specified limits. The safety aspect of TSP-based flash powder was
tested for its impact and friction sensitivity. To understand the thermal behavior of the TSP-based flash powder, TG analysis
and DSC were performed and compared with existing flash powder composition. The results showed that TSP could be a
perfect substituent for sulfur and could play a vital role in the making of eco-friendly (Green) crackers.
Keywords Tamarind · Flash powder · Thermal analysis · Sensitivity · Noise level · Green crackers
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in the paper container are the steps followed for making Experimental
the bijili crackers. There are a lot of options to improve the
performance of flash powders like changing their composi- Materials and methods
tion [7], addition of new chemicals [11] and reducing the
particle sizes [12]. Burning of fireworks releases gases like (i) Tamarind seed power
SO2, NOx, and C Ox, suspended particles, and several met-
als ions/oxides of aluminum, manganese, and cadmium, TSP is obtained from tamarind seed of tamarind fruit (Tama-
as pollutants which pollute the environment [5, 13] and rindus indica). The tamarind seed weighs about 40–44% of
create serious health hazards [3, 14]. tamarind fruit, widely grown in India with an annual growth
The recreational atmospheric pollution [15, 16] due to of about 300,000 tons [23, 24]. The tamarind seed is a solid
bursting of firecrackers during festival seasons like Diwali waste [25] obtained as a by-product of tamarind pulp due
[1] (India), Lantern festival [3] (Beijing, China), Guy to the huge annual growth of tamarind fruit. The tamarind
Fawkes or Bonfire Night [4, 17] (London, UK), and Yan- seed was crushed to fine powder and used in flash powder
shui Festival [2] (Taiwan) was very high, and all the con- to reduce the usage of sulfur. The ultimate analysis [26] of
centrations of the pollutants are above the permissible lim- TSP revealed that TSP can be used as a fuel because of the
its. Due to the presence of sulfur in flash powders used for high value of mass percentage of carbon (47.76%) and oxy-
making firecrackers, the emission of S O2 gas by bursting gen (42.39%). The TSP contains polysaccharides, tannins,
firecrackers during Diwali was many folds than the per- proteins and having a gross calorific value of 21 MJ kg−1
missible limits given by Central Pollution Control Board [23]. In this study, the percentage of TSP replaced for sulfur
(CPCB), India, and World Health Standards. In recent in flash powder was 5% and 10%, and the properties of TSP-
years (last 10 years), the emission of S O2 in some major based flash powder were tested and compared with normal
cities during Diwali was 2–6 times higher in Delhi [18], flash power samples. The 5% and 10% of TSP-based flash
5 times higher in Kolkatta [19], and 6.59 times higher in powder samples were carefully chosen for study because a
Lucknow [20]. In 2003, the emission of S O2 in Hisar city minimum of 10% and a maximum of 17% sulfur are required
of Haryana, India, was increased tenfold at few sites. In to impart good cracking characteristics for flash powders
Nagpur [21] city, during the year 2012 Diwali, the amount used for making crackers [6]. The tamarind seeds were
of SO2 in the ambient air of National Environmental Engi- brought from a local supplier, Sathur, Tamil Nadu, India.
neering Research Institute (NEERI) residential colony was The tamarind seeds were oven-dried at 110 °C for 12 h to
70.33 µg m−3 which was higher than the permissible limit remove moisture [23]. Then, they were grinded in the flour
of 60.0 µg m −3 (24 h) in the residential and rural areas mill and finally a fine powder form was obtained.
standard given in National Ambient Air Quality Standards
of India (NAAQS), CPCB, India. Recently (2017–2018), (ii) Preparation of normal and TSP‑based flash powder
in India, the developments of green cracker through gov-
ernment and industries collaborative funded projects are The raw materials used for making flash powder such as
underway to lower the emission of SO2 gases. In addition, potassium nitrate (KNO3), aluminum (Al), and sulfur (S) of
any change in flash powder composition could affect the fireworks industrial grade were purchased from local mar-
safety and prone to accidents because of self-ignition [22] ket, Sivakasi, Tamil Nadu, India. The physical properties of
during its storage and handling. The objective of this study these raw materials used for making flash powder used in
is to reduce the amount of sulfur without comprising the bijili crackers are listed in Table 1. The raw materials were
noise and safety performance of normal flash powder by thoroughly mixed well in non conducting rubber mat surface
replacing it with tamarind seed powder (TSP). and sieved by a brass sieve with Mesh No. 325-ASTM &
Table 1 Details of raw Name of chemical powders Standard test sieve Average particle Purity/%
material used for flash powder size/nm
manufacturing Mesh no. IS designa-
tion/μm
ASTM BS
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Experimental analysis of tamarind seed powder‑based flash powder composition for eco‑friendly… 3011
350-BS for three to five times to obtain uniform homogene- Table 2 Chemical composition of FPS used in fabricating bijili crack-
ous flash powder mixture. The molar quantity of the ingre- ers
dients used in the flash powder making was summarized in Sample name Chemical composition/%
a table, and table data were provided as supplementary data
Potassium Alu- Sulfur (S) Tamarind seed
for further reference. nitrate minum powder (TSP)
(KNO3) (Al)
Fabrication of bijili cracker
FPSN 60 20 20 –
FPS5 60 20 15 5
Bijili crackers were made by using the prepared flash powder
FPS10 60 20 10 10
samples in the fireworks industry in Sivakasi, India. About
300 mg of the prepared flash powder sample was tightly
filled in a paper tube of rolled using a newsprint grade paper
of 45–50 g m−2 to make a cylindrical shape of length 4.0 cm,
diameter 0.6 cm and having a paper sheet thickness of
0.5 mm (approximately 4 plies). The paper tube dimension
was as per Petroleum and Explosive Safety Organization
(PESO) standards [5]. At the top of the paper tube, a fuse
(made by charcoal powder) of length 4 cm with 6–9 s delay
was fitted at the center position for the ignition of the bijili
cracker. The base of the paper tube was sealed by a mixture
of a binding agent made by clay and dextrin particles to
avoid any leakage of flash powder.
In this work, three different sets of bijili crackers were
made using different flash powder composition. The first
set of bijili crackers were made using normal flash power
composition which was 60% K NO3, 20% Al, and 20% S
which is mainly used in bijili crackers in India. The second
set and third set of bijili crackers were prepared by replac-
ing the normal flash powder of bijili cracker with 5% and
10% of tamarind seed powder (TSP). The second set of
bijili crackers were made using 5% TSP by replacing 5%
of sulfur in the normal flash powder composition, and its
Fig. 1 A sample of bijili crackers made using 5% or 10% TSP-based
composition was 60% KNO3, 20% Al, 15% S, and 5% TSP. flash powder samples (FPS5 and FPS10)
The third set (bijili) was made using 10% TSP by replac-
ing 10% of sulfur in the normal flash powder composition,
and its composition was 60% KNO3, 20% Al, 10% S, and Fourier transform infrared spectroscopy (FTIR)
10% TSP. The percentage of TSP was chosen according to
study the impact of TSP in flash powder composition with The FTIR spectrum of TSP was recorded in the range of
respect to noise, sensitivity, and emission performance and 4000–400 cm−1 with a resolution of 4 cm−1 using RXI Perki-
compared with the normal flash power composition used nElmer FTIR spectrophotometer to ensure the purity of TSP.
in bijili cracker. For easy understanding, the normal flash
powder composition was labeled as FPSN and the 5% and X‑ray diffraction (XRD)
10% TSP (replaced with sulfur) flash powder was labeled as
FPS5 and FPS10. The chemical composition of flash powder The XRD pattern of TSP was obtained using Bruker Eco D8
samples (FPS) used in the fabrication of bijili crackers and Diffractometer in the 2θ range of 10°–100° using Cu anode
for noise, sensitivity, and thermogravimetry (TG) analysis is having K-alpha beam of 1.5424 Å (average of K-alpha1 and
listed in Table 2. These flash powder samples (FPSN, FPS5, K-alpha2 beam) at a voltage of 40 kV and current of 20 mA
and FPS10) of mass 300 mg were used for the fabrication of to ensure the purity of TSP.
bijili crackers, and it was used for noise level studies. The
samples of bijili crackers made using 5% and 10% TSP are Particle size analysis
shown in Fig. 1. About 10–15 mg of as prepared FPSs was
used for sensitivity test and for thermogravimetry analysis The particle size of the tamarind seed powder and flash
about 4–5 mg was used. powder sample was measured using Shimadzu SALD 2300
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model particle size analyzer. Particle size distribution is cal- The following procedure was adopted to measure the
culated using the light intensity distribution pattern of scat- limiting energy of the FPSs. 10 mg of bijili cracker sam-
tered light generated from sample particles. During analysis, ple was taken and kept in the bottom anvil. Top anvil is
the holder temperature was maintained at 25 °C with disper- placed above the mixture sample. The impacting mass of
sion medium viscosity as 0.896 mPa s. 2 kg was set at the required height and dropped from the
predetermined height. Before releasing the impact mass,
Morphology analysis the extreme caution was taken to ensure the straightness of
the sample position. The spark sensor was also placed near
The morphology of the flash powder sample was observed the bottom anvil. During the impact test, the distance at
through JSM-7900F Schottky field emission scanning elec- which the explosion occurred was observed and recorded.
tron microscope. To observe the morphology of the tamarind The same procedure was repeated for other heights to
seed powder, a small amount of tamarind seed powder is determine the limiting energy of the FPSs. The test was
taken and placed over the carbon tape for conduction and it conducted thrice, and the average value of the experiment
was slightly pressed to bind with the tape. The carbon tape is was reported.
placed in the SEM platform, and images were recorded using The friction sensitivity of the FPSs was tested in the
electron acceleration of between 15 and 20 kV. friction test apparatus (Fig. 3) STANAG 4487 as per the
standard procedure dictated in—EN 13631-3 & BAM [27].
Mechanical sensitivity analysis Friction sensitivity of the FPSs was observed by placing
~ 15 mg of FPS in the porcelain plate made of technical
The impact sensitivity of the FPSs was measured as per porcelain with dimension 25 × 25 × 5 mm. The porcelain
German Federal Institute for Testing Materials, Bundesan- pin was placed over the sample. The porcelain pin was also
stalt für Materialforschung und –prüfung (BAM)-[UN Test made of technical porcelain of length 15 mm and diameter
Series.3] method by using impact sensitivity tester supplied of 10 mm with a spherical tip on both ends having 10 mm
by Electro Ceramic (P) Ltd, India. A fixed mass of 2 kg was as a radius of curvature. The porcelain plate was securely
dropped from different heights to record the safest impact placed in the assembly. The assembly with the porcelain
energy of FPSs without explosion. The impact sensitivity plate was moved to and fro along a direction over the fixed
of the FPSs was expressed in terms of limiting energy. The porcelain pin for a distance of about 10 mm with a speed
instrumental setup used to determine the limiting energy is of 141 rpm. Several trials were conducted to exactly iden-
shown in Fig. 2. tify the loading range.
Fig. 2 The instrumental setup used for measuring limiting energy of Fig. 3 Friction tester used for measuring friction sensitivity of the
the FPSs FPSs
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Experimental analysis of tamarind seed powder‑based flash powder composition for eco‑friendly… 3013
Thermal analysis 40
TSP
35
The FPSs were analyzed for their thermal properties to study
the mass loss during heating in thermogravimetry (TG) 30
Transmittance/arb. units
analysis and differential scanning calorimetry (DSC) using
DSC instrument (PerkinElmer, Model: DSC 4000 System), 25
10
Noise level testing
5
Noise level test was carried out as per the rules of noti-
fication of Petroleum and Explosives Safety Organization, 0
4000 3500 3200 2800 2400 2000 1600 1200 800 400
Govt. of India. It was measured by four noise level monitors
Wavenumber/cm–1
(Fig. 4) using Model no. 824L (Make: Larson and Davis,
USA), and the measurement procedures are discussed in
Fig. 5 FTIR spectrum of TSP
[4]. The sound level is measured in decibel unit, denoted
as dB. dBA and dBC are the two common ways to express
the sound level in dB units, where A and C correspond to by the FTIR spectrum of TSP [23, 30, 32] and by 1.27698
the type of filter used in measuring the sound level. Filter d value from XRD [30] reported earlier. The particle size
A is used to measure the midrange frequencies, and filter C distribution and morphology of all the raw materials used
is used to measure the low and high frequencies of sound. for making FPS are shown in Figs. 7 and 8. The particle size
The noise produced by crackers at a distance of 4 m from distribution of these raw materials used for making flash
the point of bursting is recorded in dB(AI) and dB(C) values powder is one of the important parameters in firework indus-
[28]. The dB(AI) value indicates the risk of noise (impact tries regarding safety [12] in handling and noise efficiency
noise)-induced hearing loss [29] in humans, and dB(C) indi- [7] of the crackers produced from them. From Fig. 7, the
cates the peak noise level. average particle size of all the raw materials used for making
flash powder was 0.05 μm (50 nm).
The noise level generated by FPSs used to make bijili
Result and discussion crackers is shown in Table 3. The bijilis made using FPS5
and FPS10 generated noise less than the specified noise level
The FTIR spectrum and XRD of the TSP are shown in 125 dB(AI) and 145 dB(C). The noise level was reduced
Figs. 5 and 6. TSP mainly contains polysaccharide with fats, by 14 dB(AI) and 12.7 dB(C) for FPS5 when compared to
tannins, proteins, and amino acids in minimum proportion
[30, 31]. The TSP sample was pure, and it was confirmed
1200
TSP
1000
Intensity/arb. units
800
600
400
200
0
10 20 30 40 50 60 70 80 90 100
2θ /°
Fig. 4 Measuring the noise level of bijili cracker using noise level
meter Fig. 6 XRD of TSP
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Experimental analysis of tamarind seed powder‑based flash powder composition for eco‑friendly… 3015
at the height of 0.18 m. Similarly, the limiting energy cal- imparted good cracking characteristics by keeping the limit-
culated for FPS10 was 4.905 J (above which ignition occur) ing energy same for FPSN and FPS5.
calculated at the height of 0.25 m. The FPSN, FPS5, and Friction sensitivity test of all the FPS is tabulated in
FPS10 were considered to be very sensitive chemical mixture Table 5. The friction sensitivity test limits the value of fric-
according to the Andrejev and Beljajev (1965) which states tion load, above which the explosion will occur due to fric-
that if the limiting energy is less than 5.0 J, then it could be tion [27]. From Table 5, the flash occurred for FPSN and
classified as a very sensitive chemical mixture under class FPS5 at friction load of 360 N, but not for FPS10 at the
IV. The addition of 5% TSP instead of sulfur did not affect friction load of 360 N. In addition, from Table 5, it was
or alter the limiting energy of FPS5 and it behaved as the very clear that the flash did not occur for all the FPS at the
FPSN composition. On contrary, the addition of 10% TSP friction load of 324 N. The safe friction load for FPSN and
instead of sulfur affected and increased the limiting energy FPS5 was 324 N, above which explosion will occur. But, for
from 3.532 to 4.905 J. From these observations, FPS10 had FPS10, the safe friction load was 360 N above which explo-
less impact sensitivity (limiting energy value) than FPS5 and sion may occur. This showed that the addition of 5% TSP
FPSN, and the impact sensitivity (limiting energy value) of did not affect the performance of FPS5 when compared to
FPSN and FPS5 was same. The reason for this was due to FPSN. On contrary, the addition of 10% TSP increased the
the 10% of sulfur in FPS10 which was in the lower speci- safe friction load from 324 N to 360 N when compared to
fied limit [6] (minimum 10% and maximum 17% of sulfur) FPSN and FPS5. The increase in percentage of TSP in flash
required to impart good cracking characteristics for the FPS powder increased the limiting energy (impact test) and safe
and increased the limiting energy when compared to FPS5 explosion load (friction test), thereby increasing the safety
and FPSN. But, 20% and 15% of sulfur in FPSN and FPS5 limit during its handling.
Table 4 Limiting impact energy Flash powder Load (m)/kg Height (h)/m Number of trial Limiting energy/J
of FPSN, FPS5, and FPS10 samples
1 2 3 4 5 6
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Mass loss/%
85
may due to the Archimedes effect which happened during 80
the start of the analysis. Before increasing the temperature,
75
the fluid (flow of N 2 gas) forces the sample pan upward
which leads to an increase in mass of about ~ 0.9 g during 70
FPSN 360 X X ✓ – – –
324 X X X X X X
FPS5 360 X ✓ ✓ – – –
324 X X X X X X
FPS10 360 X X X X X X
324 X X X X X X
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hemicelluloses are present along with cellulose. The pres- 1546 cm−1 corresponding to C=O stretching confirmed the
ence of cellulose and hemicelluloses was confirmed from presence of ketone carbonyl present in hemicelluloses. The
the FTIR spectrum of TSP. In Fig. 9, the presence of a high small peak at 1745.58 cm−1 was due to the presence of ester
intense strong broad peak at 3348 cm−1 corresponding to OH C=O stretching which in turn confirmed the presence of
group [37–39] stretching vibration of glucose and another triglyceride and phospholipids present in the TSP [38]. Due
high intense strong sharp peak at 1158 cm−1 correspond- to 10% of TSP in FPS10, the volume of gases produced dur-
ing to glycoside linkage [40, 41] confirmed the presence of ing devolatilization (around 63% to 68% of volatile matter
cellulose in TSP. In addition, the strong peak at 1082 cm−1 [25, 26] in TSP)and decomposition was more than the FPS5
corresponding to C–O–C stretching vibration [35] also con- which had only 5% of TSP. The noise level produced by the
firmed the presence of cellulose in TSP. The absence of a FPS10 was higher than the FPS5 due to sudden expansion
peak at 1635 or 1638 cm−1 due to OH bending of adsorbed of more volume of gases produced by TSP in FPS10 during
water [39] showed that the TSP was completed dried and its decomposition reaction.
resistant to hydrolysis because cellulose is crystalline (Fig. 6 The DSC curve coupled with TG helped to analyze the
shows 2θ peak value at 19.35°) and resists hydrolysis. The transitions involved in the thermal decomposition of FPSN,
highest absorbance of OH and C–O was found for cellulose, FPS5, and FPS10. The DSC curve of FPSN, FPS5, and
and on the other hand, the highest absorbance of C=O was FPS10 is shown in Fig. 10. Thermal events of FPSN, FPS5,
meant for hemicelluloses [35]. The presence of medium peak and FPS10 during DSC analysis are summarized in Table 8.
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In Fig. 10, for the FPSN, the first small dip at 115 °C corre- as mentioned for the FPSN. This implies that the process
sponded to the endothermal effects associated with the phase occurring in FPS5 and FPS10 was same as the FPSN. In
transition of sulfur [42, 43]. The second and third small dip addition to the first large peak as in FPSN, FPS5 and FPS10
of FPSN at 135.43 °C and 325.42 °C corresponds to the had two more small board peaks at ~ 350 °C and at ~ 420 °C.
endothermic phase transition of KNO3. Generally, the melt- These two small exotherm peaks appeared mainly due to the
ing point of K NO3 takes place at 334 °C. The fourth broad thermal decomposition of the hemicelluloses and celluloses
dip in the DSC curve of FPSN was due to the endothermic present in the TSP [45–47]. In Fig. 10, these exotherm peaks
reaction associated with the melting of aluminum in the tem- are easily observed in FPS10 than in FPS5 due to 10% of
perature range of 800–900 °C [44]. The curved fall associ- TSP in FPS10, whereas the FPS5 had only 5% of TSP.
ated with dips in the DSC curve indicated that the volatile The onset, end, decomposition temperature, and heat
melting process was taking place, i.e., the liquid FPS evapo- of decomposition reaction of FPSN, FPS5, and FPS10 are
rates, and it was confirmed by the large change in mass in the summarized in Table 9. For FPSN, the decomposition reac-
TG curve. The large peak at 270.75 °C in the DSC curve was tion started at 226.43 °C (onset temperature) and ended at
due to the high exothermic thermal decomposition reaction 281.06 °C (end temperature). The decomposition tempera-
of FPSN. The first, second, third, and fourth dip in the DSC ture (peak position) of FPSN was 270.75 °C. Similarly, for
curve of FPS5 and FPS10 appeared at the same temperature FPS5 and FPS10, the decomposition temperature started at
218.55 and 204.96 °C and ended at 267.56 and 263.61 °C,
respectively. The decomposition temperature of FPS5 and
FPS10 was at 260.26 and 255.90 °C. The onset tempera-
Exo 550 ture is an indication of the thermal stability of the energetic
FPSN
500 70
60
FPS5 materials. Generally, the higher the onset temperature, more
FPS10
450 the thermal stability is which means that high temperature
Heat flow/mW
50
40
400 30
20
is required for the material for the thermal decomposition
350 10 reaction. On comparing the onset temperature of FPSN and
Heat flow/mW
0
300 – 10 FPS5, the FPS5 has 5% TSP and the onset temperature was
– 20
250 100 150 200 250 300 350 7.88 °C (3.48%) lesser than FPSN. Similarly, on compar-
200
Sample temperature/°C ing the onset temperature of FPS10 with FPSN and FPS5,
150 for the FPS10 with 10% TSP, the onset temperature was
100 21.47 °C (9.48%) lesser than FPSN and 13.59 °C (6.22%)
50 lesser than FPS5. From this, it was very clear that increasing
0
the percentage of TSP powder in FPSs decreases the onset
– 50
temperature and thereby decreases their thermal stability
100 200 300 400 500 600 700 800 900 1000 [48]. This may be due to the presence of high volatile mat-
Sample temperature/°C ter [25, 26] present in TSP. On comparing the decomposi-
tion temperature of FPSN and FPS5, the decomposition tem-
Fig. 10 DSC curve of FPSN, FPS5, and FPS10 perature was 10.49 °C lesser than FPSN. Similarly, for the
Table 8 Thermal events of FPSN, FPS5, and FPS10 during DSC analysis
Sample Dips/peaks Number Temperature/°C Thermal event
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Table 9 The onset, end, and decomposition temperature for FPSN, first peak, a small bump can be identified and it clearly
FPS5, and FPS10 revealed that it was a melting process with decomposi-
Sample Temperature/°C ∆H/J g−1 tion. The small second endothermic peak following the
bump at around 320 °C was due to the transformation of
Onset End Decomposition
aluminum to first metastable χ-Al 2O 3. The broad third
FPSN 226.43 281.06 270.75 − 1440.48 endothermic peak at around 800 to 900 °C was due to
FPS5 (5% TSP) 218.55 267.56 260.26 − 814.22 the formation of second metastable κ-Al2O3 [49]. Similar
FPS10 (10% TSP) 204.96 263.61 255.90 − 536.24 peaks were observed for FPS5 and FPS10. For FPS5 and
FPS10, two new peaks appeared at ~ 310 °C and ~ 450 °C
as shown in Fig. 11. These two new peaks were due to the
release of volatile hydrocarbon during devolatilization of
4 FPSN
FPS5 hemicelluloses (at ~ 310 °C) and cellulose (at ~ 450 °C)
FPS10
2
present in TSP.
0
DTG/mg min–1
Conclusions
–2
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