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Abstract
Polyolens (PE, PP and PS) were pyrolysed in a uidised-bed reactor on kilogram scale at 510 C. Pyrolysis products were analysed with GC, GC/MS and other methods. It was shown that valuable products, mostly aliphatic waxes, are received from polyolens. It was also investigated if mixtures of dierent polyolens (PE, PP, PS) interact with each other in uidised bed pyrolysis
yielding dierent pyrolysis products than received from the pure, individual polyolens. The same polymer mixtures were also
analysed using a pyro-GC/MS-device. # 2000 Elsevier Science Ltd. All rights reserved.
Keywords: Pyrolysis; Polyolens; Polyethylene; Polypropylene; Polystyrene; Fluidised bed reactor; Pyro-GC/MS
1. Introduction
In 1997 the total consumption of plastics was
27,281,000 t in the European Union. More than 10 million t were polyethylenes (HDPE/LDPE/LLDPE) and
nearly 6 million t were polypropylene (PP). Polyvinyl
chloride (PVC) and polystyrenes (PS/EPS) followed
with a consumption of 4.6 million or 2.7 million t
respectively. Forty-two per cent of all plastics were used
for packaging [1].
A huge amount of plastic waste is collected from german households every year by the DSD (Duales System
Deutschland). After sorting out the PVC by specic
weight in a water bath a polyolen mixture remains
(polyolen light fraction). This mixture consists mostly
of polyethylene (PE), polypropylene (PP) and polystyrene (PS). A possible way to recycle these plastics is
to pyrolyse them in a uidised bed reactor (Hamburg
Pyrolysis Process). This well established and optimised
technical pyrolysis process was developed in the 1970s [2].
At 700 C aromatics and olenic gases are the main
products from polyolen feedstock [3]. When the uidising gas is replaced by steam, olens are the main
products [4,5].
0141-3910/00/$ - see front matter # 2000 Elsevier Science Ltd. All rights reserved.
PII: S0141-3910(00)00131-2
374
375
Table 1
Process parameters of uidised bed pyrolysis experiments
Experiment
#01
#02
#03
#04
#05
#06
#07
#08
#09
100
100
60
40
40
60
90
10
100
90
10
54
36
10
100
5133
5163
4656
4:20
826.2
5.6
3.70
5121
5161
4474
5:15
952.4
4.6
4.40
5102
5132
4773
3:45
1066.7
4.3
4.80
5101
5161
4681
3:55
1021.3
4.1
4.9
5122
5172
4451
3:42
973.0
4.1
4.90
5103
5143
4582
3:48
1052.6
4.2
4.85
512 1
5141
4711
3:55
1020.4
4.0
5.00
5131
5151
4701
3:50
1043.5
4.1
4.95
5142
5152
4701
3:52
967.7
3.9
5.10
246.1
1054.5
2208.3
9.1
3518
3500
18
100.5
127.2
523.4
4331.8
8.5
4991
5000
9
99.8
169.5
682.1
3123.8
4.5
3980
4000
20
99.5
167.7
708.8
3079.5
7.1
3933
4000
37
99.1
72.7
550.3
2959.0
1.3
3583
3600
17
99.5
222.0
1224.7
2506.2
3.1
3956
4000
44
98.9
177.2
1378.0
2434.8
3.0
3993
4000
7
99.8
103.2
892.5
2939.0
5.6
3940
4000
60
98.5
83.6
270.2
3135.8
6.2
3496
3500
4
99.9
Input material
% PE
% PP
% PS
Table 2
Pyro-GC/MS-experiment parameters
Device
510 C
Macherey & Nagel, Optima-1-TG
25 m length, 0.32 mm diameter,
0.1 mm lm
Helium 5.0, 60 kPa
1:5
80 C (5 min),
3 C/min>360 C (30 min)
About 50 mg
Ionisation method: electron
impact ionisation (EI)
Ionisation voltage: 70 eV
Detector voltage: 1.4 V
Mass range: 30-700 m/z
Scan interval: 1 s
Scanspeed: 1000 amu/sa
Carrier gas
Split ratio
Temperature program
Input
MS-parameters
376
The pressure was controlled manually using the compressor valves. The compressor pumped the gas, which
was nearly free of higher hydrocarbons after passing the
separation unit, into the uidised bed again. The excess
gas was burned in a are after its volume, pressure and
temperature was measured. Gas samples were taken in
regular intervals. Process parameters are shown in Table 1.
Table 3
Mass balances of experiments at 510 C on PE/PP mixtures (in wt%)
Experiment
Input%
Sum Gases
PE
PP
Hydrogen
Methane
Ethane
Ethene
Propane
Propene
n-Butane
i-Butane
n-Butenes
i-Butene
Butadiene
#02
#09
#03
#04
#01
#06
100
0
100
0
60
40
40
60
0
100
0
100
0.026
0.19
0.34
0.46
0.44
0.53
0.22
0.0039
0.35
0.032
0.035
2.6
0.022
0.19
0.31
0.44
0.36
0.53
0.17
0.0029
0.32
0.028
0.033
2.4
0.011
0.33
0.58
0.54
0.41
1.8
0.12
0.025
0.26
0.42
0.037
4.5
0.029
0.34
0.67
0.39
0.45
2.3
0.060
0.064
0.53
0.26
0.018
5.1
0.015
0.42
0.90
0.31
0.45
3.5
0.023
0.059
0.16
1.0
0.0081
6.8
0.0081
0.34
0.96
0.26
0.43
3.8
0.021
0.053
0.10
1.0
0.0064
6.9
i-, n-C5
i-, n-C6
i-, n-C7
i-, n-C8
i-, n-C9
==>2,4-Dimethylheptene
i-, n-C10
i-, n-C11
i-, n-C12
i-, n-C13
n-C14,15+i-C14,15,16,17
n-C16,17+i-C18,19,20
Sum aliphatics
==>Naphtenes
==>Alkanes
==>Alkenes
==>Dienes
Aromatics
Not identied or detected
Sum Oils (bp< 300 C)
0.65
1.2
1.0
0.67
0.65
0.84
0.77
0.68
0.63
1.5
1.8
10.4
0.47
3.0
6.6
0.78
0.0071
2.7
13.2
0.57
1.2
1.1
0.66
0.70
0.84
0.82
0.71
0.73
1.5
1.9
10.6
0.50
3.1
6.8
0.76
0.033
3.0
13.7
1.7
1.9
1.0
0.88
3.8
2.6
1.0
0.73
0.94
0.69
2.6
1.7
16.8
0.65
3.5
11.8
1.5
0.018
2.6
19.4
2.3
2.0
0.86
0.77
5.1
3.3
0.91
0.63
0.98
0.71
2.6
1.6
18.5
0.57
3.9
13.0
1.6
0.0042
4.8
23.2
3.5
3.0
1.1
0.99
10.0
7.1
1.0
0.63
1.5
0.80
4.2
1.4
28.2
0.73
4.6
22.0
1.6
0.021
8.5
36.7
3.2
3.0
1.1
0.86
10.7
8.9
1.1
0.64
1.6
0.78
4.3
1.4
28.6
0.72
4.3
22.7
1.6
0.031
6.8
35.4
0.63
2.1
2.3
2.3
2.4
2.5
2.4
2.4
2.4
2.4
2.4
24.0
0.59
2.5
2.7
2.6
2.8
2.9
2.9
2.9
2.8
2.9
2.9
28.5
0.73
2.1
2.2
2.2
2.2
2.3
2.3
2.3
2.3
2.3
2.3
23.2
0.72
2.1
2.0
2.3
2.2
2.2
2.2
2.1
2.2
2.2
2.2
22.4
1.7
2.2
1.7
2.0
1.9
2.1
2.0
2.0
2.0
2.0
2.0
21.6
1.1
2.5
1.9
2.0
1.9
2.0
1.8
1.5
1.8
1.8
1.8
20.2
60.0
0.17
100.0
55.2
0.18
100.0
52.8
0.11
100.0
49.1
0.18
100.0
34.6
0.26
100.0
37.3
0.078
100.0
377
378
Table 4
Mass balances of experiments at 510 C on PE/PS mixtures (in wt%)
Experiment
Input%
Sum Gases
PE
PS
Hydrogen
Methane
Ethane
Ethene
Propane
Propene
n-Butane
i-Butane
n-Butenes
i-Butene
Butadiene
n-C5
n-C6
n-C7
n-C7
n-C9
n-C10
n-C11
n-C12
n-C13
n-C14
n-C15
n-C16
n-C17
Sum Aliphatics
==>Naphtenes
==>Alkanes
==>Alkenes
==>Dienes
Benzene
Toluene
Styrene
Ethylbenzene
a-Methylstyrene
Other Aromatics
Sum Aromatics
Not identied or detected
#02
#09
#05a
#05
100
0
100
0
100*
0
90
10
0.026
0.19
0.34
0.46
0.44
0.53
0.22
0.0039
0.35
0.032
0.035
2.6
0.022
0.19
0.31
0.44
0.36
0.53
0.17
0.0029
0.32
0.028
0.033
2.4
0.65
1.2
1.0
0.67
0.65
0.84
0.77
0.68
0.63
0.70
0.80
0.86
0.92
10.4
0.47
3.0
6.6
0.78
0.0071
0.0071
2.7
13.2
0.57
1.2
1.1
0.66
0.70
0.84
0.82
0.71
0.73
0.77
0.73
0.90
0.97
10.6
0.50
3.1
6.8
0.76
0.0093
0.024
0.033
3.0
13.7
0.81
1.4
1.2
0.80
0.84
0.95
0.91
0.81
0.81
0.87
1.0
1.3
1.4
13.2
0.65
3.9
8.3
1.0
13.2
0.73
1.3
1.1
0.72
0.76
0.86
0.82
0.73
0.73
0.78
0.91
1.2
1.3
11.9
0.58
3.5
7.5
0.90
0.017
1.1
5.2
0.36
0.34
0.47
7.5
2.4
21.8
0.63
2.1
2.3
2.3
2.4
2.5
2.4
2.4
2.4
2.4
2.4
24.0
0.59
2.5
2.7
2.6
2.8
2.9
2.9
2.9
2.8
2.9
2.9
28.5
0.47
3.1
3.2
3.4
3.3
3.4
3.3
3.3
3.3
3.3
3.3
33.6
0.43
2.8
2.9
3.1
3.0
3.0
3.0
3.0
3.0
3.0
3.0
30.2
60.0
0.17
100.0
55.2
0.18
100.0
50.4
0.041
100.0
45.3
0.037
100.0
0.027
0.22
0.37
0.54
0.40
0.65
0.21
0.0027
0.41
0.046
0.039
2.9
0.025
0.20
0.33
0.49
0.36
0.59
0.19
0.0024
0.37
0.042
0.035
2.6
379
380
Table 5
Mass balances of experiments at 510 C on PP/PS mixtures (in wt%)
Experiment
Input%
Sum Gases
PP
PS
#01
#06
#07a
#07
100
100
100*
90
10
Hydrogen
Methane
Ethane
Ethene
Propane
Propene
n-Butane
i-Butane
n-Butenes
i-Butene
Butadiene
0.015
0.42
0.90
0.31
0.45
3.5
0.023
0.059
0.16
1.0
0.0081
6.8
i-C5
i-C6
i-C7
i-C8
i-C9
==>2,4-Dimethylheptene
i-C10
i-C11
i-C12
i-C13
i-C14
i-C15,16,17
i-C18,19,20
Sum Aliphatics
==>Naphtenes
==>Alkanes
==> Alkenes
==>Dienes
Benzene
Toluene
Styrene
Ethylbenzene
a-Methylstyrene
Other Aromatics
Sum Aromatics
Not identied or detected
0.0038
0.31
0.77
0.25
0.31
3.1
0.019
0.044
0.11
0.88
0.0059
5.8
0.0034
0.28
0.69
0.23
0.28
2.8
0.017
0.040
0.10
0.79
0.0053
5.2
3.5
3.0
1.1
0.99
10.0
7.1
1.0
0.63
1.5
0.80
0.18
4.0
1.4
28.2
0.73
4.6
22.0
1.6
0.021
0.021
8.5
36.7
3.2
3.0
1.1
0.86
10.7
8.9
1.1
0.64
1.6
0.78
0.19
4.1
1.4
28.6
0.72
4.3
22.7
1.6
0.031
0.031
6.8
35.4
3.1
2.8
1.0
0.86
10.5
9.3
1.0
0.61
1.5
0.81
0.20
4.1
1.5
28.1
0.60
4.1
22.4
1.6
3.8
31.8
2.8
2.5
0.92
0.77
9.4
8.4
0.90
0.55
1.3
0.73
0.18
3.7
1.4
25.3
0.54
3.7
20.2
1.4
0.0074
0.38
7.1
0.11
0.29
0.41
8.3
5.1
38.7
1.7
2.2
1.7
2.0
1.9
2.1
2.0
2.0
2.0
2.0
2.0
21.6
1.1
2.5
1.9
2.0
1.9
2.0
1.8
1.5
1.8
1.8
1.8
20.2
1.3
2.7
1.9
2.0
2.3
1.9
1.8
1.9
2.0
2.0
2.0
21.8
1.1
2.4
1.7
1.8
2.1
1.7
1.7
1.7
1.8
1.8
1.8
19.6
34.6
0.26
100.0
37.3
0.078
100.0
40.5
0.084
100.0
36.4
0.075
100.0
0.0081
0.34
0.96
0.26
0.43
3.8
0.021
0.053
0.10
0.99
0.0064
6.9
381
Fig. 5. (a) Gas-chromatograms of light wax fractions from PP/PS-experiments (uidised bed); (b) GCs of light wax fractions from PP/PS-experiments (uidised bed) ne structure.
382
Table 6
Mass balances of experiments at 510 C on PE/PP/PS mixtures (in wt%)
Experiment
Input%
Sum Gases
PE
PP
PS
Hydrogen
Methane
Ethane
Ethene
Propane
Propene
n-Butane
i-Butane
n-Butenes
i-Butene
Butadiene
i-, n-C5
i-, n-C6
i-, n-C7
i-, n-C8
i-, n-C9
==>2,4-Dimethylheptene
i-, n-C10
i-, n-C11
i-, n-C12
i-, n-C13
n-C14,15+i-C14,15,16,17
n-C16,17+i-C18,19,20
Sum Aliphatics
==>Naphtenes
==>Alkanes
==>Alkenes
==>Dienes
Benzene
Toluene
Styrene
Ethylbenzene
a-Methylstyrene
other aromatics
Sum Aromatics
Not identied or detected
#03
#08a
#08
60
40
60*
40*
54
36
10
0.011
0.33
0.58
0.54
0.41
1.8
0.12
0.025
0.26
0.42
0.037
4.5
0.012
0.32
0.59
0.50
0.46
1.8
0.13
0.027
0.26
0.38
0.028
4.5
0.011
0.29
0.53
0.45
0.41
1.7
0.11
0.024
0.23
0.34
0.025
4.1
1.7
1.9
1.0
0.88
3.8
2.6
1.0
0.73
0.94
0.69
2.6
1.7
16.8
0.65
3.5
11.8
1.5
0.012
0.0065
0.018
2.6
19.4
1.7
1.8
0.91
0.75
4.0
2.7
0.94
0.65
1.0
0.69
2.5
1.8
16.7
0.54
3.7
11.6
1.4
1.5
18.3
1.5
1.6
0.82
0.67
3.6
2.4
0.85
0.59
0.90
0.62
2.3
1.6
15.1
0.49
3.3
10.5
1.2
0.014
0.50
6.3
0.15
0.29
0.47
7.7
3.6
26.4
0.73
2.1
2.2
2.2
2.2
2.3
2.3
2.3
2.3
2.3
2.3
23.2
1.1
2.4
2.3
2.3
2.4
2.4
2.3
2.3
2.3
2.3
2.3
24.4
0.96
2.2
2.0
2.1
2.1
2.1
2.1
2.1
2.1
2.1
2.1
22.0
52.8
0.11
100.0
52.7
0.16
100.0
47.4
0.14
100.0
383
Table 7
PE/PP mixtures pyrolysed at 510 C on a pyro-GC/MS (in TIC%)a
Pyro-GC/MS-Experiment
#3
#17
#21
#10
#18
#9
#19
#8
#11
#7
#12
#15
#1
#2
100:0
46
100:0
41
100:0
63
80:20
26
80:20
48
60:40
31
60:40
45
40:60
38
40:60
33
20:80
35
20:80
30
20:80
48
0:100
106
0:100
59
29.1
2.3
31.4
3.1
2.2
2.4
2.3
2.2
2.5
2.9
3.0
3.6
3.4
55.6
32.0
2.3
34.3
3.2
2.0
2.1
2.0
2.9
2.3
2.6
2.6
2.8
3.2
56.9
30.4
2.4
32.8
3.1
2.2
2.5
2.7
3.4
3.1
2.9
3.6
3.4
3.7
59.7
29.9
2.2
32.1
2.5
2.1
2.2
2.3
2.7
2.7
2.8
3.4
4.2
3.7
57.0
25.8
1.8
27.6
2.4
2.0
2.1
2.3
3.2
2.8
3.3
3.7
4.5
4.7
53.9
23.3
2.4
25.6
3.7
2.7
3.1
2.9
3.2
3.2
3.4
3.5
3.7
4.0
55.0
25.8
1.8
27.6
2.6
2.1
2.5
2.4
2.7
3.1
3.6
3.7
4.4
4.5
54.7
19.3
3.4
22.7
3.0
3.2
2.5
3.0
2.7
3.1
3.6
3.6
3.5
3.6
50.9
20.3
2.9
23.2
2.6
2.5
2.8
2.8
3.5
3.2
3.4
3.8
4.5
4.6
52.2
16.4
3.7
20.1
2.8
2.9
2.9
3.2
3.7
4.0
4.3
4.4
4.9
5.0
53.1
13.8
3.8
17.6
3.1
3.1
3.6
3.5
3.6
3.9
4.2
4.6
4.7
4.8
51.8
12.8
3.1
15.9
2.9
2.9
3.4
3.6
4.2
4.2
4.3
4.8
5.2
5.6
51.5
11.2
2.2
13.4
2.7
2.8
3.2
3.4
3.7
3.8
4.1
4.4
4.4
4.7
45.8
8.8
1.8
10.7
2.6
2.8
3.1
3.6
3.7
4.3
4.3
4.7
4.7
4.8
44.5
40.9
39.9
36.7
39.3
41.4
41.1
40.8
45.6
43.2
42.0
43.4
42.9
49.5
50.6
100
100
100
100
100
100
100
100
100
100
100
100
100
100
384
Table 8
Pyro GC/MS-experiments at 510 C on PE/PS-mixtures (results in TIC%)a
Pyro-GC/MS-Experiment #1
Input ratio PE:PS
Input [mg]
#2
#6
#20
#13
#22
#24
R PS-Pyrolysis Products
1.9
2.0 16.9 13.1 15.8
H2, n-C1-15 11.2
8.8 11.5 14.9 24.3 23.4 24.8
n-C16-17
2.2
1.8
2.2
1.9
2.0
1.5
1.8
Oils, Gases (bp < 300 C) 13.4 10.7 13.7 16.9 26.3 25.0 26.6
2.7
2.6
2.6
2.2
2.0
1.9
1.6
n-C18-19
n-C20-21
2.8
2.8
2.9
2.6
1.9
1.9
2.1
n-C22-23
3.2
3.1
3.2
2.7
2.3
2.2
2.1
n-C24-25
3.4
3.6
3.6
3.1
2.6
3.1
2.5
3.7
3.7
3.8
3.7
2.7
3.7
2.7
n-C26-27
n-C28-29
3.8
4.3
4.2
4.1
3.0
3.5
2.8
n-C30-31
4.1
4.3
4.5
4.0
3.2
3.7
3.3
n-C32-33
4.4
4.7
4.8
4.4
3.3
4.1
3.3
4.4
4.7
5.1
4.8
3.7
4.0
3.7
n-C34-35
n-C36-37
4.7
4.8
5.4
4.9
3.7
4.3
4.1
Light Waxes
37.1 38.7 40.1 36.4 28.4 32.4 28.3
(300 C < bp < 500 C)
Heavy Waxes
49.5 50.6 44.3 44.7 28.4 29.6 29.4
(bp > 500 C, > n-C37)
Total
100 100 100 100 100 100 100
a
#1
#2
#6
#20
#13
#22
#24
100:0
100:0
90:10*
90:10*
50:50*
50:50*
50:50*
106
59
42
40
40
74
30
polystyrene decomposition products not considered
only products due to PE-pyrolysis shown
11.2
2.2
13.4
2.7
2.8
3.2
3.4
3.7
3.8
4.1
4.4
4.4
4.7
37.1
8.8
1.8
10.7
2.6
2.8
3.1
3.6
3.7
4.3
4.3
4.7
4.7
4.8
38.7
11.7
2.3
14.0
2.6
2.9
3.3
3.7
3.9
4.3
4.6
4.9
5.2
5.5
40.9
15.2
2.0
17.2
2.3
2.6
2.8
3.2
3.7
4.2
4.1
4.5
4.9
5.0
37.2
29.3
2.4
31.7
2.4
2.3
2.7
3.1
3.3
3.6
3.8
4.0
4.4
4.5
34.1
27.0
1.7
28.7
2.1
2.1
2.5
3.6
4.3
4.1
4.2
4.7
4.6
5.0
37.2
29.4
2.1
31.5
2.0
2.5
2.5
2.9
3.3
3.4
3.9
4.0
4.4
4.8
33.6
49.5
50.6
45.2
45.6
34.2
34.1
34.9
100
100
100
100
100
100
100
385
Table 9
Pyro GC/MS-experiments at 510 C on PP/PS-mixtures (results in TIC%)a
Pyro-GC/MS-Experiment #3
#17 #21 #4
#5
#14 #16 #21
Input ratio PP:PS
100:0 100:0 100:0 90:10 90:10 50:50 50:50 50:50
Input [mg]
46
41
63
30
62
43
43
34
R PS-pyrolysis products
H2, C1-17
i-C18-20
Oils, Gases (b.p < 300 C)
i-C21-23
i-C24-26
i-C27-29
i-C30-32
i-C33-35
i-C36-38
i-C39-41
i-C42-44
i-C45-47
i-C48-50
Light Waxes
(300 C < bp < 500 C)
Heavy Waxes
(bp > 500 C, >i-C50)
Total
a
#3
#17
#21
#4
#5
#14
#16
#21
100:0 100:0 100:0 90:10* 90:10* 50:50* 50:50* 50:50*
46
41
63
30
62
43
43
34
polystyrene decomposition products not considered
only products due to PE-pyrolysis shown
27.0
33.4
1.5
34.9
3.0
1.6
1.9
2.2
2.2
1.9
2.2
2.0
2.3
2.1
21.4
29.1
2.3
31.4
3.1
2.2
2.4
2.3
2.2
2.5
2.9
3.0
3.6
3.4
27.7
32.0
2.3
34.3
3.2
2.0
2.1
2.0
2.9
2.3
2.6
2.6
2.8
3.2
25.8
30.4
2.4
32.8
3.1
2.2
2.5
2.7
3.4
3.1
2.9
3.6
3.4
3.7
30.6
30.8
1.8
32.5
2.8
2.1
2.5
2.2
2.4
2.7
3.2
3.3
3.1
3.1
27.4
29.4
2.1
31.5
2.8
2.0
2.5
2.2
2.2
2.1
2.4
3.1
2.8
3.5
25.7
38.6
2.7
41.3
3.3
3.0
2.5
3.7
3.2
2.4
3.4
3.2
3.0
3.2
30.9
40.9
2.8
43.7
4.2
2.3
2.6
2.5
2.6
2.0
2.2
2.5
3.0
3.2
27.1
45.8
2.1
47.9
4.1
2.2
2.7
3.0
3.0
2.6
3.0
2.7
3.2
2.9
29.3
40.9
39.9
36.7
40.1
42.8
27.7
29.1
22.9
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
4. Conclusions
Mixed polyolens can be converted by uidised bed
pyrolysis at 510 C into valuable oils and waxes, which
can be used as feedstock in petrochemical processes.
The amount usable in a steam cracker (<500 C boiling
point) is 50 wt.% when using PE-feed and 70 wt.% when
using PP-feed. The amount usable from PE/PP-mixture
can be calculated on basis of these gures, because their
pyrolysis products can be calculated additionally.
When adding 10% PS to either PE or PP or a PE/PPmixture the distribution of products fractions does not
change signicantly apart from additional PS degradation products. This observation is contradictory to
other pyrolysis methods [912].
But when adding PS to PP the peak distribution of
the waxes changes signicantly, although its amount
remains constant: The formation of diene-waxes is
favoured at i-C30 and higher. But this fact will surely
have little eect when this product fraction is fed into a
steam cracker.
By using a pyro-GC/MS-analyser it was shown that
there is a mixing inuence of PS on the other two poly-
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