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UTS - 140310180011 - Effect of Temperature On Biochar Product Yield From Selected
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ORIGINAL PAPER
Received: 28 February 2012 / Accepted: 12 April 2012 / Published online: 22 May 2012
Ó Springer Science+Business Media B.V. 2012
123
312 Waste Biomass Valor (2012) 3:311–318
[5, 9, 23, 25, 29]. Product distribution is often a function of Materials and Methods
heating rate, residence time and maximum reaction tem-
perature, hence different pyrolysis techniques have been Three tropical biomass: Apa wood (A. africana), Iroko
utilized to promote the yield of either the solid (carbon- wood (M. excelsa), and palm kernel shell (PKS) (E.
ization), liquid (fast pyrolysis, flash pyrolysis, ablative guineensis) were utilized in this study on the basis of
pyrolysis) or the gaseous residues (gasification). Charcoal availability, abundance and non-economic utilization of
is a highly porous residue of microcrystalline graphite that their wastes. The wood wastes were collected from two
is left behind in a pyrolysis process. Its energy density sawmills in Akure while the PKS was obtained from
(Qchar) is enhanced thermally within 28.7 B Qchar B Okitipupa, in Nigeria. The wood wastes were processed
34 MJ/kg compared to wood of 20 B Qwood B 26.5 MJ/kg into pin chips (approximately 10 9 10 9 60 mm3) while
[14, 17]. It has lightweight, higher energy density, strong the PKS was utilized as received. 10 kg each of the feed-
reducing and highly reactive properties that makes it more stocks were oven dried to constant weights at 103 ± 2 °C
desirable as industrial and domestic fuel than its parent per kg by applying ASTM: E 871 standard test methods for
stock. moisture removal.
Charcoal has strong reducing properties. It combines
very readily with O and S in metallic ores of aluminum,
bronze, copper, manganese, nickel, iron and silicon, and
produce pure metal extract when heated. It is the fuel used Experimentation
in blast furnaces before the advent of coke [6]. It is an
excellent industrial fuel for forging operations, water and Oven dried (0.5 kg batches, 3 replicates per treatment)
air purification (activated carbon), producer gas generation were pyrolyzed in a custom built fixed–bed reactor [30].
and fireworks manufacturing [12]. Charcoal based iron Three pyrolysis products: charcoal (solid fuel), bio-oils
industry still exists in a number of countries. Brazil’s (liquid fuel), and pyrogas (non-condensable gases) were
charcoal based pig iron industry is considered as the big- collected and the yields of each recorded. Pyrolysis
gest in the world. Malaysia and Argentina are among other experiments were conducted at 400, 500, 600, 700, and
significant producers [14]. Charcoal is used for the pro- 800 °C.
duction of chemicals such as: calcium carbide, carbon The moisture content of the selected materials and
disulfide, silicon carbide, sodium cyanide and various char derivatives were determined by using METTLER
pharmaceuticals [12, 20, 32]. It is also used for soil TOLEDO HB 43-S Halogen, moisture analyzer. The standard
amendments, C sequestration and helps to mitigate the test method for the Analysis of Particulate Wood Fuels was
effect of green house gas on the environment and in the adopted in determining the volatile (VM) and the ash content
preparation of biofertilizer [18, 26, 27]. Most of the char- for the various species and their derived char [2].
coal used in blast furnaces is made from hard wood species
and its use in iron smelting is highly profitable in countries FC ¼ 100 %ðMC þ VM þ Ash contentÞ ð1Þ
that have extensive forests but deficient in coking coal. -1
The concentration (mg kg ) of the inorganic elements
Charcoal is generally acknowledged to be a better reduc-
(in the biomass ash was determined by energy dispersive
tant than coke but there are practical difficulties in oper-
X-ray fluorescence spectroscopy (ED-XRFS MiniPAL 4
ating very large blast furnaces with charcoal in the iron and
Model). C, H, and N contents were determined in a LECO
steel mills [12]. However, charcoal low S content, high C
CHN Analyzer (Model: CHN-1000). The S analysis was
to ash ratio, relatively few unreactive inorganic impurities,
also determined with a ‘LECO Sulphur Determinator
stable pore structure, high surface area, good reduction
MODEL SC 132 and O by difference (Eq. 2). All
ability and its almost smokeless combustion ability gives it
elemental analyses were performed at the International
an edge over coal, coke and other petroleum fuels.
Institute of Tropical Agriculture Ibadan, Oyo state of
The quality of charcoal for industrial and domestic uti-
Nigeria.
lization is often determined by its physiochemical charac-
teristics [12]. These include the MC, FC, ash content, %C, O ¼ 100 %ðC þ H þ N þ S þ AshÞ ð2Þ
S content and energy value (HHV). The aim of this work
was to investigate the thermochemical reaction for charcoal
(carbonization) with respect to temperature severity, heat- Results and Discussion
ing rate, residence time, reaction environment and biomass
species to produce products of varying physiochemical The residual yields of char from selected biomass feed-
characteristics. The quality of the derived charcoals for stock decreased with increasing pyrolysis temperatures
industrial and domestic applications is also considered. (Table 1, Fig. 1), as the volatiles were liberated (Fig. 2).
123
Waste Biomass Valor (2012) 3:311–318 313
50 CApa = -0.0288T + 50.66 Apa Table 2 Variance ratios (F-calculated) from various ANOVA tables
R² = 0.98 for char residues
45 CIroko = -0.0166T + 41.12 Iroko
F value
Char yield (%)
R² = 0.98
PKS
40 CPKS = -0.0191T + 45.66 Species treatment 46.331*
R² = 0.96
Carbonization temp. (C. Temp) 130.859*
35
Interaction (Species * C. Temp) 5.536*
2
30 *Significant (p \ 0.05), R = 0.957
25
350 450 550 650 750 850 decreased significantly with increasing carbonisation tem-
Temperature (°C) perature and residence time among all the species and vice
versa. The degree of biomass carbonisation is therefore a
Fig. 1 Plot of char yield against temperatures for selected lignocel-
precursor for determining the yield and the quality of solid
lulosic biomass
residue (charcoal) produced in a pyrolysis reaction, as the
volatiles evolves (Fig. 2) and material shrinks.
50 The ash content of the parent stocks were: 1.08 % for
VM Apa = -0.1117T + 85.798 Apa apa wood, 0.82 % for iroko wood and 2.23 % for PKS
Volatile matter yield (%)
40 VM Iroko = -0.0365T + 34.346 Iroko (Table 3). It fell within the range of 0.5–2.7 % for tropical
VM PKS = -0.0562T + 44.168 PKS trees reported by [7, 10]. Temperature interaction produced
30 corresponding material shrinkage as volatile matter evolves
across species as reported by [8]. The ash content increased
20
with temperature severity across selected biomass as
reported by [18]. The ash content for the derived char for
10
all the species ranged between 1.31 % for apa wood at
0 400 °C to 8.20 % for iroko wood at 800 °C. This fell
350 450 550 650 750 850 within the range of 3–10 % reported by [1, 12] for charcoal
Temperature (°C) intended for use in blast furnaces. This suggests that the
derived biochar from the temperature range of 600–800 °C
Fig. 2 Plot of volatile matter yield against temperatures for selected
for all species can favorably serve as metallurgical char-
lignocellulosic biomass
coals. It was also observed that the mineral matter in the
The effect of temperature on selected biomass and char biomass feedstock has a level of influence on the charcoal
yield across species is highly significant (p \ 0.05) yield across species as reported by [1]. Higher ash content
(Table 2). This implies that all the species reacted to in parent stocks influenced higher biochar yield (Fig. 1,
temperature significantly (Table 3) but degrade differently Table 3) for PKS, while lower ash content produced less
to produce char residues at corresponding temperatures biochar yield for iroko wood at all temperatures. However,
(Table 1, Fig. 1). Figure 1 indicated that the starting apa wood biochar yield (Fig. 1, Table 3) followed the same
materials produced a yield of 39.4 % of char at 400 °C and pattern at lower temperature, but deviated at higher tem-
27 % at 800 °C for apa wood; 34.1 % at 400 °C and perature and the reason (s) for this not yet clear.
27.8 % at 800 °C for iroko wood and 38.8 % at 400 °C and The volatile matter (VM) of the oven dried parent stock
30.9 % at 800 °C for PKS. This also suggests a difference was 77.9 % for apa wood, 78.3 % for iroko wood and
in the degree of organic polymerisation of the selected 79.3 % for PKS (Table 3). Apa wood degraded and liber-
2
materials. Tables 1 and 2 shows that char residual yield ated volatiles at the rate of oVM
oT = -0.1 g/°C (R = 0.9) to
123
314 Waste Biomass Valor (2012) 3:311–318
APA ASH (%) 1.08 1.31 ± 0.01e 1.59 ± 0.02d 1.94 ± 0.01c 2.21 ± 0.01b 2.59 ± 0.02a
e d c b
IROKO 0.82 4.89 ± 0.02 6.38 ± 0.49 7.45 ± 0.01 8.03 ± 0.02 8.20 ± 0.01a
PKS 2.23 4.07 ± 0.02e 5.19 ± 0.02d 6.17 ± 0.01c 6.26 ± 0.01b 6.39 ± 0.11a
e d c b
APA FC (%) 21.06 56.38 ± 0.23 63.44 ± 0.09 87.33 ± 0.78 94.02 ± 0.19 95.36 ± 0.05a
e d c b
IROKO 20.93 74.65 ± 0.48 77.35 ± 0.06 81.54 ± 0.04 84.38 ± 0.02 85.13 ± 0.03a
e d c b
PKS 18.45 73.65 ± 0.51 78.54 ± 0.07 83.4 ± 0.02 91.64 ± 0.05 92.3 ± 0.09a
a b c d
APA VM (%) 77.86 42.31 ± 0.22 34.97 ± 0.10 10.73 ± 0.78 3.77 ± 0.19 2.05 ± 0.04e
IROKO 78.25 20.46 ± 0.46a 16.49 ± 0.08b 11.01 ± 0.03c 7.58 ± 0.01d 6.66 ± 0.03a
PKS 79.32 22.28 ± 0.51a 16.27 ± 0.06b 10.43 ± 0.01c 2.09 ± 0.05d 1.29 ± 0.11e
Values are: Means ± Standard Deviation. Values in a row with the same superscript are not significantly different from each other
* Parent stock
produce charcoal of 42.3 % mean value volatiles matter [12, 15]. In this work, all charcoal derivatives with the
VM at 400 °C and 2.05 % at 800 °C. Iroko wood liber- exception of apa wood (56.38 % FC obtained at 500 °C)
ated volatiles at the rate of oVM 2 are of the quality and met the required grade for metal-
oT = -0.04 g/°C (R = 0.95)
to produce charcoal of 20.5 % VM at 400 °C and 6.66 % lurgical applications as reported by FAO [12]. A general
at 800 °C, while PKS liberated volatiles at the rate of trend of progressive increase in FC is observed for all
oVM 2 samples across temperatures. The temperature range of
oT = -0.06 g/°C (R = 0.96) to produce charcoal of 600–800 °C seem good for producing metallurgical char-
22.3 % VM at 400 °C and 1.29 % at 800 °C (Fig. 2, coals in the reactor. This study reveals that severity in
Table 3). The VM of the charcoal produced across species temperature improves FC content of biomass derived
fell within the range of charcoal intended for domestic charcoals and by extension its thermo-chemical properties.
cooking (20–30 %), except for apa wood derived charcoal The effect of heat on the elemental (C, H, O, S and N)
at 400 °C, although 40 % VM is still marginally accept- content of the starting materials and charcoal derivatives
able. The VM of the charcoals produced between 600 and (Table 4) was investigated to determine the effect of
800 °C for all the species fell within ‘‘good-quality’’ temperature on them. The initial %C of the oven dried apa
charcoal, intended for use as metallurgical charcoal which wood was 58.2 %. It was upgraded by temperature to
often contains 10–15 % VM [1, 11, 12]. Table 3 suggest 82.7 % at 400 °C and 96.1 % at 800 °C. Also, %C for
that temperature is a precursor in thermochemical reac- iroko wood was 57.3 %, it upgraded to 80.2 % at 400 °C
tions, VM is species specific and the rate of biomass deg- and 91.1 % at 800 °C while that of PKS was 46.8 % and
radation is accelerated by temperature severity (p \ 0.05). upgraded to 81.9 % at 400 °C and 93.0 % at 800 °C
This further suggests that temperature severity drives off (Table 4). A general trend of %C upgrade by temperature
volatiles to produce valuable charcoal with high energy was observed across selected materials and the derived
content and of smokeless quality. charcoals tend to approach absolute carbon at elevated
The value of FC content of the char residues increased temperatures (Tables 4, 5). This study therefore suggests
with severity in temperatures (Table 3) and corresponding that upgrading the %C in charcoal by temperature effect
decrease in charcoal yield in all the experiments (Fig. 1). will simultaneously address its energy content. Biochar
The FC for the starting materials were: 21.1 % for apa derivatives with appreciable %C would serve as alternate
wood 20.9 % for iroko wood and 18.5 % for PKS. The FC fuel to its non-renewable energy cousins in some industrial
for the derived charcoal ranged from 56.4 % (400 °C) to applications.
95.4 % (800 °C) for apa wood, 74.7 % (400 °C) to 85.1 % The %S was low across the oven dried biomass species
(800 °C) for iroko wood, and 73.7 % (400 °C) to 92.3 % making them environmentally friendly (Table 4). The S
(800 °C) for PKS. This fell within the range of 50–95 % of content for apa wood, iroko wood and PKS were 1.1, 1.4
FC content of charcoals reported by FAO [12]. The upper and 0.5 %S respectively. The mean value %S contained
limit of that range was attained by apa wood at 800 °C. in the char derivatives range from 0.23 % at 400 °C to
The fixed C content of 60 B FC C 80 % in charcoal 0.04 % at 800 °C for apa wood; 0.03 % at 400 °C to
is considered good for firing blast furnaces while 0.02 % at 800 °C for iroko wood; and 0.36 % at 400 °C to
75 B FC C 80 % is considered excellent for its operations 0.3 % at 800 °C for PKS. The available %S in the char
123
Waste Biomass Valor (2012) 3:311–318 315
APA C (%) 58.2 82.74 ± 0.07e 86.48 ± 0.05 88.3 ± 0.24 94.51 ± 0.03b 96.1 ± 0.02
e
IROKO 57.33 80.22 ± 0.02 82.03 ± 0.02 83.0 ± 0.03 90.47 ± 0.05b 91.12 ± 0.03a
PKS 46.77 81.89 ± 0.02e 82.19 ± 0.02 87.57 ± 0.20 92.46 ± 0.13b 93.01 ± .00
APA N (%) 0.31 0.65 ± 0.01 0.77 ± 0.02 0.83 ± 0.02 0.97 ± 0.01 1.08 ± 0.01
IROKO 0.29 1.16 ± 0.01 1.22 ± 0.01 1.35 ± 0.03 1.42 ± 0.01 1.47 ± 0.02
PKS 0.63 0.84 ± 0.05 0.87 ± 0.01 0.97 ± 0.01 1.05 ± 0.01 1.13 ± 0.41
APA H (%) 6.24 3.27 ± 0.02 0.61 ± 0.02 0.47 ± 0.01 0,37 ± 0.01 0.16 ± 0.01
IROKO 6.53 0.097 ± 0.01a 0.09 ± 0.02 0.07 ± 0.01 0.05 ± 0.02 0.1 ± 0.00
PKS 16.53 0.88 ± 0.01 0.61 ± 0.02 0.44 ± 0.01 0.06 ± 0.01 0.00 ± 0.00
APA O (%) 33.07 11.8 ± 0.69 10.36 ± 0.03 8.31 ± 0.19 1.87 ± 0.01 0.037 ± 0.01e
IROKO 33.63 13.33 ± 0.02a 9.7 ± 0.5 7.95 ± 0.04 0.53 ± 0.02 0.04 ± 0.01
PKS 33.34 11.58 ± 0.67a 8.82 ± 3.45 3.22 ± 2.42 0.28 ± 0.23 0.03 ± 0.03
APA S (%) 1.1 0.23 ± o.01 0.18 ± 0.03 0.14 ± 0.03 0.07 ± 0.02 0.04 ± 0.01
b
IROKO 1.40 0.30 ± 0.01 0.23 ± 0.2 0.14 ± 0.01 0.17 ± 0.01 0.02 ± 0.01
PKS 0.50 0.36 ± 0.15 0.32 ± 0.01 0.12 ± 0.25 0.11 ± 0.25 0.3 ± 0.02
* Parent Stock
Table 5 Variance ratios (F-calculated) from various ANOVA tables for ultimate analysis
Carbon Nitrogen Hydrogen Sulphur Oxygen
derivatives approach zero as carbonization temperature 7,933.33 mg kg-1 for iroko wood and 12,833.33, 7,400,
increases. This suggests that temperature severity is a 5,566.67 mg kg-1 for PKS. The influence of the temperature
factor for modifying biomass physiochemical structure to on the elements with low concentrations (minor elemental
produce environmentally benign fuel. The H and O content constituents of the ash): P, Na, Mn, Fe, Zn and Cu (Table 6), is
reduced with temperature while that of N and ash increased observed to have followed the same trend. This suggests that
with temperature (Tables 3, 4). The O content of the temperature severity is a means of upgrading ash elemental
derived char approaches zero at elevated temperatures concentrations relative to its yield (Table 3).
(Table 4) across all samples. This therefore, suggests that The analysis of variance in (Table 7) revealed a sig-
temperature severity drives off O and reduce biomass nificant (p \ 0.05) interaction between biomass and tem-
internal ballast to near zero at temperature around 800 °C, perature. The rate of change of the constituent elemental
to produce C rich biochar. concentration in the ash with temperature among the
The inorganic elements of Ca, Mg, and K were the major selected biomass, was significantly different (p \ 0.05)
elements that were present in the ash. They have the following except for Ca. Pyrolysis temperature seems to have pro-
concentrations respectively: 5,600, 2,300, and 1,100 mg kg-1 duced the same effect on the concentration of Ca content
for apa wood; 7,800, 3,400, and 3,800 mg kg-1 for iroko among the selected biomass, hence it was statistically
wood; 3,600, 1,800, and 1,100 mg kg-1 for PKS (Tables 6, insignificant (p [ 0.05). However, the reason for the
7). The elements were upgraded by temperature at 400 °C to peculiarity of Ca at producing similar variation effect
8,800, 4,833.33, and 2,200 mg kg-1 for apa wood, 18,000, with temperature, among the species is not very clear. The
8,500, 6,633.33 mg kg-1 for iroko wood and 6,833.33, 4,000, presence of heavy metal concentrations was not detected in
3,000 mg kg-1 for PKS. Temperature interaction at 800 °C the ash of any of the materials. This suggests that biomass
further improved the concentrations to 15,300, 7,533.33, and ash is non-pollutant but contain beneficial macronutrients
4,533.33 mg kg-1 for apa wood, 23,566.67, 9,666.67, and for soil remediation and improved fertility as reported by
123
316
123
Table 6 Mean and standard deviation of the inorganic constituents in the ash of selected lignocellulosic biomass
Pyrolysis temp (°C) Concentration (mg/kg)
Ca Mg K P Na Mn Fe Zn Cu
Apa wood
P/Stk 5,600 2,300 1,100 16.913 21.081 17.316 18.216 8.216 2.372
400 °C 8,800 ± 360.56 4,833.33 ± 115.47 2,200 ± 200 31.15 ± 0.22 28.32 ± 1.96 32.88 ± 4.48 27.09 ± 5.67 16.53 ± 1.04 4.84 ± 1.60
500 °C 10,400 ± 435.89 5,400 ± 100 2,633.33 ± 115.47 41.56 ± 1.42 32.44 ± 0.64 39.80 ± 1.07 35.64 ± 0.63 18.91 ± 1.09 7.19 ± 0.21
600 °C 12,466.67 ± 1,209.68 6,466.67 ± 208.17 3,066.67 ± 152.75 51 ± 1.16 35.77 ± 1.58 47.15 ± 1.89 39.17 ± 2.07 20.53 ± 0.66 7.84 ± 0.21
700 °C 14,366.67 ± 493.29 7,000 ± 100 3,900 ± 100 57.88 ± 1.41 46.80 ± 2.16 51.43 ± 1.59 46.22 ± 0.09 23.09 ± 0.27 8.36 ± 0.07
800 °C 15,300 ± 200 7,533.33 ± 152.75 4,533.33 ± 115.47 62.14 ± 0.89 51.08 ± 1.14 57.19 ± 1.08 50.30 ± 0.78 25 ± 0.16 9 ± 0.03
Iroko wood
P/Stk 7,800 3,400 3,800 21.3 38.143 23.168 27.128 19.117 2.172
400 °C 18,000 ± 100 8,500 ± 529.15 6,633.33 ± 152.75 70.43 ± 1.48 69.88 ± 1.41 69.59 ± 1.43 58.45 ± 1.42 25.37 ± 0.67 3.95 ± 0.07
500 °C 19,200 ± 264.58 8,400 ± 100 7,000 ± 100 77.43 ± 0.61 74.61 ± 0.78 69.04 ± 0.62 59.35 ± 0.78 26.56 ± 0.76 4.03 ± 0.07
600 °C 21,733.33 ± 2,592.94 9,100 ± 100 7,066.67 ± 152.75 80.33 ± 0.67 76.26 ± 0.89 66.09 ± 5.31 61.06 ± 1.08 28.09 ± 1.54 4.20 ± 0.18
700 °C 21,756.67 ± 706 9,533.33 ± 57.74 7,566.67 ± 115.47 83.30 ± 3.02 79.50 ± 1.4 70.90 ± 1.4 62.29 ± 3.70 31.09 ± 0.99 4.55 ± 0.07
800 °C 23,566.67 ± 503.32 9,666.67 ± 152.75 7,933.33 ± 152.75 89.66 ± 1.45 82.60 ± 5.16 79.45 ± 2.02 61.73 ± 1.74 34.26 ± 0.31 4.92 ± 0.13
PKS
P/Stk 3,600 1,800 1,100 27.186 12.816 13.25 20.081 8.15 2.077
400 °C 6,833.33 ± 152.75 4,000 ± 100 3,000 ± 100 49.01 ± 0.86 26.02 ± 0.51 21.46 ± 1.14 36.83 ± 0.96 17.51 ± 0.81 4.53 ± 0.15
500 °C 8,100 ± 200 5,266.67 ± 152.75 3,800 ± 100 55.88 ± 1.18 29.87 ± 2.22 25.84 ± 0.54 39.34 ± 1.08 19.39 ± 0.63 5.06 ± 0.10
600C 9,200 ± 264.58 6,366.67 ± 416.33 4,233.33 ± 115.47 61.39 ± 1.43 33.50 ± 1.16 27.63 ± 1.59 42.14 ± 1.88 22.30 ± 0.74 6.03 ± 0.09
700 °C 11,733.33 ± 850.49 6,933.33 ± 152.75 6,000 ± 1,734.94 64.16 ± 0.20 40.28 ± 0.84 30.70 ± 0.79 52.07 ± 1.06 26.22 ± 0.83 6.17 ± 0.17
800 °C 12,833.33 ± 305.51 7,400 ± 100 5,566.67 ± 152.75 67.88 ± 0.41 50.440.80 31.40 ± 1.31 55.05 ± 0.28 30.57 ± 1.02 5.40 ± 0.41
P/Stk parent stock, PKS palm kernel shell
Waste Biomass Valor (2012) 3:311–318
Waste Biomass Valor (2012) 3:311–318 317
Table 7 Variance ratios (F-calculated) from various ANOVA tables for Ash constituents
Calcium Magnesium Potassium Phosphorus Sodium Manganese Iron Zinc Copper
Species 722.002* 964.635* 284.777* 2,320.780* 2,196.819* 1,508.781* 410.296* 384.894* 189.873*
Temperature 76.322* 206.470* 32.399* 438.362* 163.279* 60.761* 79.194* 210.350* 31.280*
Interaction 1.188 ns 13.454* 2.478* 19.189* 8.236* 11.463* 12.627* 5.373* 8.664*
* Significant (p \ 0.05), ns not significant [ 0.05)
[26, 27]. The increasing variation of ash elemental com- characteristics which met the industrials charcoals
position with temperature among the species suggests that requirement reported by [12].
thermal degradation in pyrolysis is peculiar to biomass
polymeric constituents alone. The concentration of the Acknowledgments The Authors appreciate University of Idaho
relatively unreactive inorganic materials in the char resi- and gratefully acknowledge the funding from USDA-CSREES
dues continues to appreciate as temperature and residence Wood Utilization Research program grants (2008-34158-19486 and
time increases (Tables 1, 3 and 6). This is due to the mass 2009-34158-20170) for making the completion of this work possible.
loss engendered by the evolving volatiles as biomass
polymer chain is unzipped by heat. References
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