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CHARACTERIZATION OF POLYMERS

BY MEANS OF TG-FTIR (III)


Ekkehard Fglein and Claire Louis
NETZSCH-Gertebau GmbH, Wittelsbacherstrae 42, D-95100 Selb, Germany
NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH

DTG /(%/min)
Gram Schmidt

TG /%

0.60
395.5 C

0.00
0.50

sample:
PMMA, granule
sample mass:
5.06 mg
crucible:
Al2O3,
[1] 006-3-06-11.dt3
sample
carrier:
Al2O3 , corrosive rest.
TG
atmosphere:
nitrogen
(20 + 20 ml)
Gram Schmidt
heating rate:
20
K/min
DTG

80.0

60.0

-10.00
0.40
-20.00
0.30

-99.2 %

Absorbance Units
0.5
1.0

PMMA

Temperature of
decomposition
(DTG minimum):

1.5

10.00
100.0

391C
Main
decomposition
products:

-30.00
40.0

0.10

20.0

0.00

391.2 C

0.0

-40.00

0.0

0.20

H3C O C O
CH2 C
CH3 n

-50.00
4000

3500

3000

-60.00

2500
2000
Wavenumber cm-1

1500

1000

propionic acid,
methyl ester

Residual Mass: 0.8 % (596.8 C)


Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-11_PMMA\006-3-06-11_PMMA_392.0

100.0

200.0

300.0
Temperature /C

400.0

500.0

C:\OPUS\search\Hit858.0

PMMA

5.062 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-11_PMMA\006-3-06-11.dt3

METHACRYLIC ACID, METHYL ESTER

NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH

250.0

-0.6 %

0.25

2.5

Gram Schmidt
Flow /(ml/min)
DTG /(%/min)

TG /%

NH3

5.00

Temperature of
decomposition
(DTG minimum):

458.7 C

0.00

90.0

200.0
872.0 C

sample:
80.0
sample mass:
crucible:
sample
carrier:
70.0
atmosphere:
heating rate:

-5.00

PA66, granule
9.85 mg
[1] 006-3-06-14.dt3

-63.3 %

TG
Al2O3,
Flow (purge1)
Al2O3 Flow
, corrosive
(purge2) rest.
nitrogen
Schmidt
air
Gram
DTG
20 K/min

0.15
-10.00

150.0

873.1 C

60.0

CO2

0.20

0.10

Absorbance Units
1.0
1.5

PA66

2.0

100.0

454C

-15.00

Main
decomposition
products:

0.5

100.0
50.0

H
H O
O
N (CH2)6 N C (CH2)4 C n

-20.00
0.05
-1.4 %

-25.00

50.0

0.0

40.0
454.2 C

Residual Mass: 34.6 % (987.3 C)

30.0

0.00

4000

3500

3000

-30.00
nitrogen

20.0

0.0
100.0

200.0

300.0

400.0 500.0 600.0


Temperature /C

700.0

800.0

2500
2000
Wavenumber cm-1

1500

1000

air
Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-14_PA66\006-3-06-14_PA66_450.0
C:\OPUS\search\Hit2835.0
CARBON DIOXIDE
C:\OPUS\search\Hit2870.0
AMMONIA
C:\OPUS\search\Hit2082.0
CYCLOHEXANECARBOXYLIC ACID, METHYL ESTER

900.0

PA66

ammonia,
cyclohexane carboxylic
acid, methyl ester

9.850 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-14_PA66\006-3-06-14.dt3

NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH

DTG /(%/min)
Gram Schmidt

TG /%

80.0

60.0

0.20

sample:
ABS, plate
sample mass:
8.02 mg
[1] 006-3-06-18.dt3
crucible:
Al2O3, TG
sample carrier:
Al2Schmidt
O3 , corrosive rest.
Gram
DTG(20 + 20 ml)
atmosphere:
nitrogen
heating rate:
20 K/min

-10.00
0.15
-94.3 %

0.10

CH

453C

-20.00

Main
decomposition
product:

0.5

40.0

C N
CH2 CH n CH2 CH CH CH2
CH2
m

Temperature of
decomposition
(DTG minimum):

0.00

462.8 C

Absorbance Units
1.0
1.5

ABS

ABS (450C)
SAN (428C)

2.0

0.25

100.0

0.05

-30.00

0.00

-40.00

0.0

20.0
452.9 C

4000

3500

3000

2500
2000
Wavenumber cm-1

1500

1000

Residual Mass: 5.7 % (696.9 C)

0.0
100.0

200.0

300.0
400.0
Temperature /C

500.0

600.0

acetonitrile,
phenyl

Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-19_ABS\006-3-06-19_ABS_450.0

ABS

9.430 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-19_ABS\006-3-06-19.dt3

Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-17_SAN\006-3-06-17_SAN_428.0

SAN

10.290 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-17_SAN\006-3-06-17.dt3

C:\OPUS\search\Hit1659.0

ACETONITRILE, PHENYL-,

NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH

exo

0.00

1.0

PBT

80.0

0.25

sample:
PBT, plate
[1] 006-3-06-15.dt3
sample
mass:
9.59
mg
TG
crucible:
Al2O3,
Gram Schmidt
DTG
sample carrier:
Al
2O3 , corrosive rest.
[2] c-DTA_006-3-06-15.dt3_0.mt3
atmosphere:
nitrogen (20 + 20 ml)
c-DTA
heating rate:
20 K/min

1.00

-10.00

0.20
0.80
-93.6 %

0.15

-20.00

Absorbance Units
0.5

1.20

60.0

0.10

0.40

0.05

0.20

-40.00

20.0
0.00

-0.5

-50.00

4000

0.00
413.6 C

100.0

200.0

300.0
400.0
Temperature /C

500.0

3500

3000

2500
2000
Wavenumber cm-1

1500

1000

-0.20

Residual Mass: 6.4 % (646.7 C)

0.0

Main
decomposition
product:

0.0

-30.00

O
C O CH2 CH2 CH2 CH2 O

414C

0.60

227.9 C

40.0

-60.00

Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-15_PBT\006-3-06-15_PBT_417.0

600.0

C:\OPUS\search\Hit1078.0

BENZOIC ACID

C:\OPUS\search\Hit1726.0

TEREPHTHALIC ACID, DIBUTYL ESTER

PBT

terephthalic acid,
dibutylester

9.590 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-15_PBT\006-3-06-15.dt3

DTG /(%/min)
Gram Schmidt

TG /%

2.0

NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH, NETZSCH-Gertebau GmbH

Temperature of
decomposition
(DTG minimum):

60.0

0.00

-10.00
0.15
-20.00
-97.8 %

0.10
-30.00

40.0

Absorbance Units
1.0

0.20
sample:
[1.1] 006-3-06-17.dt3SAN, granule
TGmg
sample mass:
10.29
Gram Schmidt
O3 ,
crucible:
Al2DTG
sample carrier:
Al2O3 , corrosive rest.
atmosphere:
nitrogen (20 + 20 ml)
heating rate:
20 K/min

425C

0.5

SAN

436.0 C

80.0

1.5

100.0

Main
decomposition
product:

C N
CH2 CH n CH2

CH

0.05

-40.00

20.0

0.0

O
C

Temperature of
decomposition
(DTG minimum):

10.00
1.40

0.30

417.8 C

1.5

c-DTA /K
Gram Schmidt
DTG /(%/min)

TG /%

100.0

0.00
424.8 C

0.0

-50.00
4000

3500

3000

Residual Mass: 700.0 C, 2.2 %

100.0

200.0

300.0
400.0
Temperature /C

500.0

600.0

2500
2000
Wavenumber cm-1

1500

1000

acetonitrile,
phenyl

700.0
Y:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-17_SAN\006-3-06-17_SAN_428.0
C:\OPUS\search\Hit1659.0

ACETONITRILE, PHENYL-,

All measurements were carried out employing alumina crucibles, heating rate: 20 K/min, atmosphere: nitrogen, purge gas flow rate: 40 ml/min

SAN

10.290 | NETZSCH TG 209 F1 | Z:\Commissions\823-xxx-06\006-3-06-TG209F1-FTIR-MS\006-3-06-17_SAN\006-3-06-17.dt3

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