Journal of Analytical and Applied Pyrolysis

50 (1999) 149162
Pyrolysis of solid waste in a rotary kiln:
inuence of nal pyrolysis temperature on the
pyrolysis products
A.M. Li, X.D. Li, S.Q. Li, Y. Ren, Y. Chi, J.H. Yan,
K.F. Cen *
Institute for Thermal Power Engineering, Zhejiang Uni6ersity,
Hangzhou 310027, Peoples Republic of China
Received 14 October 1998; accepted 8 January 1999
Abstract
Temperature is one of the most important parameters in pyrolysis reaction. In present
work, an externally heated laboratory-scale rotary-kiln pyrolyser was designed and devel-
oped. The inuence of nal pyrolysis temperature (FPT) on the pyrolytic products of solid
wastes has been studied. Raising FPT caused increasing gas yield and decreasing semi-coke
yield. The average heat value of the gas also changed with FPT. The content of aliphatic
hydrocarbons in PE tar increased initially and then decreased with increasing FPT. Parallel
to this, the content of aromatic ring changed conversely. FPT had obvious inuence on the
primary and elemental analysis data of the semi-cokes. The CO
2
reactivity of the semi-cokes
also varied with the FPT. The kinetic parameters of the semi-cokes were different for the
same material at the different FPT. 1999 Elsevier Science B.V. All rights reserved.
Keywords: Solid waste; Pyrolysis; Rotary kiln; Final pyrolysis temperature; Pyrolysis products
1. Introduction
For pyrolysis of solid wastes, the rotary-kiln reactor is one of the most appropri-
ate techniques. Rotary-kiln has more advantages than the other pyrolysis technolo-
gies. Solid wastes of various shapes, sizes and heat values can be fed into a
rotary-kiln either in batches or continuously. Rotary-kiln has been widely used in
* Corresponding author. Tel.: +86-571-7951335; fax: +86-571-7951616.
E-mail address: itpe@sun.zju.edu.cn (K.F. Cen)
0165-2370/99/$ - see front matter 1999 Elsevier Science B.V. All rights reserved.
PII: S0165- 2370( 99) 00025- X
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150 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
incineration and studied by many researchers [14]. In incineration, an after-burner
often follows the kiln to guarantee the complete combustion [57]. Most kilns used
in pyrolysis are internally heated. The heat value of the produced gas is very low
and the gas has to be co-combusted with oil or natural gas in the close-by utilities
[8]. In order to improve the heat value of the produced gas and to make the gas
more widely utilized, externally heated kiln should be used [9].
Temperature is one of the most important parameters in pyrolysis reaction. The
different temperature proles cause the different yield and different characteristics
of products. Some researchers have studied the inuence of temperature on the
pyrolysic products of solid waste. Williams et al. studied the pyrolysis products of
plastic waste in a laboratory-scale-uidized bed. When the temperature varied from
500 to 700C gas yield changed from 9.79 to 88.76% and tar yield changed from
18.44 to 57.11%. As the temperature increased the amount of aromatic compounds
in the tar increased [10]. Joo-sik et al. pyrolyzed PVC in a technical-scale-uidized
bed at 638, 690 and 735C. The experiment at 690C yielded about 40% tar and
half of which consisted of benzene, toluene and xylene (BTX-aromatics). At 735C
the main product was a highly aromatized tar [11]. Napoli et al. studied the
inuences of temperature on the yield and composition of semi-coke, tar and gas by
pyrolyzing scrap tire in a laboratory-scale vertical tubular furnace at 380, 450 and
550C [12]. Rausa et al. investigated the inuence of temperature on the distribu-
tion of pyrolysis products of automobile shredder residue. Two analytical tech-
niques were used: a TGA-FTIR and the System for Thermal Diagnostic Studies
(STDS) [13]. Caballero et al. used a Pyroprobe 1000 to pyrolyze kraft lingnin at
different temperatures ranging from 500 to 900C, the yield of gaseous product was
analyzed as a function of temperature [14]. Kaminsky et al. studied the pyrolysis of
mixed polyolens in a technical-scale uidized bed reactor to yield different
products. Aromatic oil compounds with total yield of 31.4% by weight were
obtained at 700C. When the temperature was reduced below 600C aromatic
production rapidly decreased. Parallel to this, aliphatic production rose while gas
yield dropped [15,16].
In this paper, an externally heated laboratory-scale rotary-kiln pyrolyser was
designed and developed (Fig. 1). The aim of the present work was to investigate the
inuence of the nal pyrolysis temperature (FPT) on the yield and characteristics of
pyrolysis products in order to provide base data for engineering purposes.
2. Experiment
2.1. Experimental apparatus and heating method
The scheme of the laboratory- scale experimental apparatus is shown in Fig. 1.
Its main components are listed below.
Rotary-kiln
Seal
Tar condenser and reservoir
Gas sampling system
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151 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
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152 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
The length of the rotary-kiln pyrolyser is 0.450 m and its internal diameter is
0.205 m. The pyrolyser can process up to 4.5 l of feedstock in each run and its
rotation rate can range from 0.5 to 10 rpm (in present tests, the kiln rotation rate
is adjusted to 3 rpm). Three k-type thermocouples are used to record the tempera-
ture in the kiln, one is xed on the inner surface, one is immerged in the material
and the other is suspended at the center of the kiln freeboard. A 12 kW electric
furnace heats the kiln. The temperature of the kiln freeboard can be up to 850C
when the temperature of the internal surface of the furnace reaches 900C. The
sealing of the rotary-kiln is always a difcult technology, especially for pyrolyser. In
this pyrolyser, the internal pressure of the kiln is higher than the atmospheric
pressure and the hot gases must be kept in carefully. A special friction-type seal is
designed and applied and it can successfully seal the hot pyrolyser. The hot
pyrolysis gas from kiln passes through a snake-tube type condenser. Most of tar
and moisture in the gas can be condensed in the condenser. The condenser is
situated vertically and the condensed tar is collected in the reservoirs, which are
tted at the lowest position of the condenser. The pyrolysis gas then passes through
a lter that is a glass tube lled with quartz wool and the remaining tar and
moisture in the gas are retained in it. The reservoirs and the lter are weighted
before and after each test. Therefore, the amount of tar and moisture generated
during the test can be evaluated. The gas ow rate is recorded by using a total ow
meter. The gas sampler is located at the end of the system. A computer-controlled
gas-sampling device is used. The computer controls the sampling procedure by
adjusting the electrical magnet valves of the sampling balls.
The kiln lled with raw material is kept out of the furnace until the temperature
of electrical furnace is stabilized at the preset value. The FPT was varied in the
range from 550 to 850C in this study.
2.2. Analytical methods
A SP-3400 type gas chromatograph was used to analyze the components of the
gas such as H
2
, CO, CH
4
, CO
2
, O
2
, N
2
, C
2
H
4
and C
2
H
6
. A 60 cm long (3.5 mm
o.d.) GDX501 column was connected to thermal conductivity detector held at
220C. The initial temperature of column was 35C and then increased at a rate of
25C min
1
until 200C by a temperature program. Helium was used as carrier.
Besides of elemental and heat value analyses, tar samples, obtained from tar
reservoirs, were processed according to SY5119-86 standard analysis method for
the soluble organic-material in rock and for the major groups of compounds in
crude oil. n-Hexane was used to precipitate the bituminous fraction. Silica gel and
Al
2
O
3
were used as adsorbent to separate the aliphatic, aromatic and polar
compounds, respectively.
In addition to the primary and elemental analyses, the reactivity of the semi-
cokes is determined. The scheme of the determination of semi-coke reactivity is
shown in Fig. 2. Semi-coke samples of 36 mm size were put into the reaction
tube. The ratio of the reacted and the introduced CO
2
concentration was used as
the means evaluating CO
2
reactivity of semi-coke at various temperatures.
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153 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 2. Scheme of measurement system of semi-coke CO
2
reactivity: (1) electric furnace; (2) reactive tube;
(3) temperature controller; (4) Orsat apparatus; (5) CO
2
container; (6) gas tank; (7) gas cleaner; (8) dry
tower; and (9) gas owmeter.
2.3. Raw materials
In this study, the typical components of MSW, wood, PE plastic and waste tire
were used as raw materials, the primary and ultimate analyses of waste (air dried
basis) are listed in Table 1.
Table 1
Primary analysis and ultimate analysis of the raw materials (air dried basis)
Waste tire Materials Wood PE plastic
Proximate analysis (wt.%)
Moisture 0.99 14.83 0.17
Ash 19.08 2.94 0.06
62.49 99.77 Volatile matter 69.41
0 12.82 17.44 Fixed carbon
Ultimate analysis (wt.%)
Carbon 70.79 40.32 89.28
Hydrogen 6.81 4.68 13.66
0.60 0.06 Nitrogen 0.18
Sulfur 1.03 0.06 0.02
0.70 0 Oxygen 36.99
High heat value (kJ kg
1
) 29 865.8 15 833.9 37 513.2
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154 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 3. Temperature prole during pyrolysis for wood.
3. Results and discussion
Pyrolysis of the solid waste results in three kinds of products: gas, tar and
semi-coke. Pyrolysis products were studied by pyrolyzing the selected raw materials
at different FPTs. The main subjects of study are listed below.
Temperature prole in the rotary kiln
Inuence of the FPT on products yield
Inuence of the FPT on gas
Inuence of the FPT on tar
Inuence of the FPT on semi-coke
3.1. Temperature prole in the rotary kiln
Temperature is a key parameter in pyrolysis reaction, the different temperature
causes the different products yield. In the tests, the heating rate of the material is
not constant. The temperature proles of wood heated to four different FPTs are
shown in Fig. 3. At higher FPT the heating rate was higher. The kiln wall
temperature was higher than that of the material and freeboard during the whole
process, because kiln has been heated externally.
3.2. Inuence of FPT on pyrolysis products yield
The different FPT means different temperature proles and results in different
pyrolysis product yield as shown in Figs. 46. The inuence of FPT on products is
obvious. Raising FPT caused increased yield of gas and decreased yield of semi-
coke. However, for PE and wood chips, tar yield decreased as FPT increased. But
for waste tire, it increased.
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155 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 4. Inuence of FPT on pyrolysis product yields of PE.
3.3. Inuence of FPT on gas
In most cases, it is desirable to get more gas yield and higher gaseous heat value.
Although the yield of gas increased with increasing FPT, the change of the average
heat value are not the same tendency as that of the gas yield, as seen in Fig. 7. As
the FPT increases from 550 to 850C, the gas yield of PE increases more quickly
Fig. 5. Inuence of FPT on pyrolysis product yields of wood chips.
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156 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 6. Inuence of FPT on pyrolysis product yields of waste tire.
than that of wood. For PE, it has a maximum value at around of 750C, but for
wood, it varies between 9200 and 12500 kJ Nm
3
. The percentages of the raw
materials heat content in gas can be calculated according to the Eq. (1).
TC=
&
t
e
t
0
6(t)H
g
(t) dt/HHV100% (1)
where: TC, percentage of thermal content in gas (%); t
0
, start of gas volatilization;
t
f
, termination of gas production; 6(t), gas yield rate at time t (Nm
3
kg
1
min
1
);
Fig. 7. Changes of average heat value of gas with FPT.
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157 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 8. Changes of percentages of raw materials heat content in gas with FPT.
H
g
(t), gas heat value at time t (kJ Nm
3
); dt, time interval (min); and HHV, high
heat value of raw material (kJ kg
1
).
The calculated results for wood and PE are shown in Fig. 8. It shows that the
percentages of the raw materials heat content in gas increase with increasing FPT.
But this does not necessarily mean a higher FPT is absolutely benecial to gas
yield, since the pyrolysis is an endothermic reaction and the higher temperature
means more heat is needed. So it exists an optimal FPT and the optimal FPT will
be different for different kinds of raw materials, different heating methods and
different types of pyrolysis furnace. This part of study will be reported in another
paper.
Table 2
Elemental analysis of and heat value of tar
Material FPT (C) C (wt.%) H (wt.%) C/H (ratio of atom) Heat value (kJ kg
1
)
71.36 PE 10.18 550 0.54 43 126.7
41 853.1 0.56 9.32 60.07 650
8.21 0.61 62.59 41 416.7 750
850 58.87 7.16 0.64 38 033.0
Waste tire 6.14 550 0.82 60.24 36 626.0
7.59 0.63 57.48 34 006.9 650
43.65 7.71 0.47 750 28 255.3
40.12 7.94 850 0.42 22 100.9
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158 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Table 3
Analysis results of primary groups of tar compounds
Aromatic ring Material FPT (C) Bituminous (%) Aliphatic hy- Polar compounds
(%) (%) drocarbons (%)
14.00 4.47 PE 550 3.60 77.93
3.56 3.10 4.14 650 89.21
15.63 8.88 4.78 750 70.71
32.34 7.15 16.33 850 44.18
1.55 Waste tire 550 49.73 29.68 19.04
2.59 19.17 23.99 650 54.25
28.99 17.71 750 2.70 50.60
30.92 22.28 850 6.53 40.27
3.4. Inuence of FPT on characteristics of tar
Table 2 presents the analyses of element C, H and the heat value of tar produced
from PE and waste tire at different FPTs. The lower value of the atom ratio of C/H
will benet to the rene of the produced tar. In present work, the value of the atom
ratio of C/H for PE tar is between 0.54 and 0.64 and increases with the increasing
FPT and for waste tire tar it is between 0.42 and 0.82 and reduces with the
increasing FPT. With the increase of FPT the heat value of PE tar decreases,
roughly in line with the depletion of both C and H content. The heat value and C
content of waste tire tar reduces like that of PE tar, while H content increases. The
higher C content and higher heat value of PE tar than those of waste tire tar are
probably due to different structural characteristics.
Table 3 summarizes the analysis results of major groups of PE and waste tire tar
compounds at different FPTs. The content of aliphatic hydrocarbons in PE tar is
higher than that in waste tire tar, while the content of aromatic ring as well as polar
organic compounds is lower. The contents of aliphatic hydrocarbons for both PE
and waste tar increase initially and then decrease with the increase of FPT.
However, the content of aromatic ring changes conversely. It is probably because
secondary reactions are enhanced with increasing temperature, when the secondary
reactions of the parafn hydrocarbons mean cracking and conversion into small gas
molecules and aromatic rings of tars. Bituminous content enhances with increasing
FPT. Polar hydrocarbons change irregularly because of their heterogeneity.
3.5. Characteristics of semi -coke
The FPT strongly affects the chemical characteristics of semi-cokes. The primary
and ultimate analyses of semi-cokes can be used as a means to broaden understand-
ing of the pyrolysis process. The reactivity of semi-coke is in close correlation to the
subsequent gasication process, therefore the kinetics of semi-coke gasication
provides valuable data for the correct dimensioning of gasiers. The semi-cokes of
wood chips and waste tire are used as samples of the test materials. The primary
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159 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
analyses of these two kinds of semi-cokes, produced at different FPT, are listed in
Table 4. With increasing FPT, the content of volatile as well as xed carbon
decreases consistently in the semi-coke of waste tire. However, for semi-cokes of
wood chips, the volatile content decreases while xed carbon content increases
slowly. Ash content increase is related directly to devolatilization of raw materials.
In each run, the heat value of semi-coke was lower than that of raw material and
it decreased with increasing FPT. The residual content of elements in semi-cokes is
evaluated using semi-coke yield, raw material and semi-coke elemental analysis
data. Percentages of original material carbon and hydrogen under different FPTs
are shown in Figs. 9 and 10, respectively. The results show that residual carbon
content in semi-cokes of both wood chips and waste tire was reduced almost
linearly with increasing FPT. However, residual hydrogen content decreases sharply
before 750C, then it changes slowly after this. The comparison of results indicates
Table 4
Primary analysis of semi-cokes (dry basis)
Material Fixed carbon Ash (%) Volatile matter High heat value FPT (C)
(kJ kg
1
) (%) (%)
68.23 550 30 617.6 17.76 14.01 Wood chips
28 498.9 68.54 11.28 20.18 650
8.87 25 056.0 22.54 68.59 750
25 504.4 850 23.87 6.88 69.24
550 33.47 18.91 47.62 20 024.0 Waste tire
15.97 18 906.8 46.62 37.41 650
16 983.9 750 49.77 7.26 42.97
31.05 850 12 408.0 61.55 7.41
Fig. 9. Changes of percentage of raw materials C in semi-coke with FPT.
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160 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Fig. 10. Changes of percentage of raw materials H in semi-coke with FPT.
that residual content of carbon in semi-cokes of wood chips is higher than that in
waste tire. The residual contents of hydrogen in semi-cokes of the two materials are
lower than that of carbon. It implies that devolatilization of hydrogen is easier
compared to carbon. When FPT is higher than 750C (FPT), less than 10%
hydrogen is remained in semi-cokes.
CO
2
reactivity data of semi-coke for wood and waste tire are listed in Table 5. It
shows that both the FPT and the reaction temperature have obvious inuences on
the reactivity of semi-coke and the latter has greater inuence.
The reaction of CO
2
and semi-coke is a gas-solid reaction. In the test condition,
the reaction is controlled by kinetics and the Eq. (2) can be used to describe the
reaction.
Table 5
CO
2
reactivity of semi-coke for wood chips and waste tire
Material CO
2
reaction rate FPT
(C)
800C 850C 900C 950C 1000C 750C
/ 0.952 0.928 0.804 Wood 0.608 0.500 550
650 0.370 0.450 0.518 0.772 0.902 /
750 0.506 0.594 0.680 0.828 0.924 /
/ 850 0.350 0.592 0.712 0.848 0.918
0.470 0.556 0.682 550 0.830 Waste tire 0.902 0.960
0.490 0.642 0.808 650 0.888 0.956 0.978
0.490 0.688 0.760 0.850 0.908 750 0.962
0.966 0.946 0.822 0.750 850 0.636 0.390
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161 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
Table 6
Kinetics parameters of semi-coke CO
2
reactivity
E
a
kJ mol
1
tk
0
Raw materials ln(tk
0
) FPT (C) E
a
/R
9.33 Wood chips 550 9.9910
3
11.3110
3
83.1
7.9310
3
8.98 87.4 650 10.5210
3
66.7 7.40 1.6410
3
750 8.0310
3
17.2310
3
9.75 89.2 850 10.7310
3
8.64 Waste tire 550 8.7710
3
72.8 5.6310
3
6.2310
3
8.74 77.6 650 9.3410
3
65.0 7.34 1.5410
3
750 7.8210
3
82.4 9.09 850 8.8510
3
9.9110
3

dc
dt
=kc (2)
where: dc, the change of the concentration of CO
2
; dt, time interval (min); k, rate
constant of reaction (min
1
); and c, concentration of CO
2
.
Integrating Eq. (2) and based on Arrhenius law, Eq. (2) becomes:
ln[1/(1x)] =tk
0
exp( E
a
/RT) (3)
where: x, the conversion rate of CO
2
; E
a
, activation energy (kJ mol
1
); k
0
,
frequency factor; t, reaction time (min); and T, reaction temperature (K).
Taking natural logarithm gives:
ln ln[1/(1x)] =E
a
/RT+ln(tK
0
) (4)
Since the CO
2
conversion rate varies with the FPT and with the nature of the raw
material (as shown in Table 5), it is necessary to select a set of representative kinetic
parameters in applying Eqs. (3) and (4) for engineering purpose. Kinetic parameters
of several kinds of semi-coke CO
2
reactivity are listed in Table 6. The activation
energy for CO
2
reaction of wood semi-coke is slightly higher than that of scrap tire
semi-coke produced at same FPT. For the tested semi-cokes, the activation energy
rises slightly with increasing FPT except that at temperature 750C. It can be partly
explained that not only the FPT, but also secondary char formation through tar
deposition and carbonation soaking time as well determine the activation energy of
semi-coke.
4. Conclusion
The inuence of FPT on products is obvious, raising FPT causes increased yield
of gas and decreased yield of semi-coke. FPT also affects the yield and heat value
of the gas. The percentages of the raw materials heat content in gas increase with
increasing FPT.
With increasing FPT the atom ratio of C/H increases for PE tar and decreases
for waste tire tar. With increasing FPT the heat value of PE tar decreases. Both for
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162 A.M. Li et al. / J. Anal. Appl. Pyrolysis 50 (1999) 149162
PE tar and waste tire tar, the contents of aliphatic hydrocarbons increase initially
and then decrease with increasing FPT. However, the content of aromatic ring
changes conversely. With increasing FPT, polar hydrocarbon contents change
irregularly due to their diversities.
FPT has obvious inuence on the primary and elemental analysis data of
semi-coke. The CO
2
reactivity of the semi-cokes also varied with FPT. The kinetic
parameters are different for the same material at the different FPT.
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