CHEMICAL AND SPECIALITY TESTING for polymers

chemical and speciality testing

1. CHEMICAL AND SPECIALITY TESTING
Presented by :
Dr.Papiya Sen Majumder
IRMRA

2. FTIR
FOURIER TRANSFORM INFRA-RED SPECTROSCOPY
Basic Principle :
Every organic chemical undergoes atomic
disturbances or vibrations on IR irradiation at
specific frequencies, which are characteristic of
the functional groups present in it .

3. FTIR
Test method
ASTM D – 3677 –1990 (Re-approved in 1995) and
BS4181 Part-1 (1985) are the standard test methods for
Rubber - identification by Infrared spectroscopy.

4. NATURAL RUBBER
4400.04000 3000 2000 1500 1000 450.0
0.1
5
10
15
20
25
30
35
40
45
50
55
60
63.8
cm-1
%T
4330
3405
3071
2958
2925
2868
2726
1710
1643
1513
1451
1375
1154
1017
963
911
886
796
767
727
885 1370 800 1640 909 cm
-1

5. ISOPRENE RUBBER
4400.04000 3000 2000 1500 1000 450.0
0.1
5
10
15
20
25
30
35
40
45
50
55
60
63.8
cm-1
%T
4330
3405
3071
2958
2925
2868
2726
1710
1643
1513
1451
1375
1154
1017
963
911
886
796
767
727
885 1370 800 1640 909 cm
-1

6. SBR
4400.04000 3000 2000 1500 1000 450.0
0.2
5
10
15
20
25
30
35
40
45
50
55
60
65
71.6
cm-1
%T
3059
3024
2856
2730
1638
1601
1494
1376
1313
1266
1156
990
965
908
872
775
698
699 775 909 990 490 962 cm
-1

7. NITRILE RUBBER
4400.04000 3000 2000 1500 1000 450.0
0.0
5
10
15
20
25
30
34.9
cm-1
%T
4344
4256
3531
3073
2926
2854 2236
2185
1731
1668
1640
1441
1350
1308
1220
1080
1032
977
922
827
756
688
549
962 2220 917 cm
-1

8. NBR/PVC
4400.04000 3000 2000 1500 1000 400.0
0.1
5
10
15
20
25
30
35
40
45
50
56.5
cm-1
%T
4337
2928
2238 1853
1788
1775
1726
1604
1546
1458
1378
1270
1124
1072
1039
967
904
793
2220 790 cm
-1

9. HYPALON
4400.04000 3000 2000 1500 1000 450.0
0.0
5
10
15
20
25
30
35.2
cm-1
%T
4330
4257
3429
1852
1788 1720
1639
1602
1454 1376
1256
1123
1071
1001
906
813
744
909 (S) 962 990 741 720 813 695 cm
-1

10. VITON RUBBER
4400.04000 3000 2000 1500 1000 450.0
0.1
5
10
15
20
25
30
35
40
45
50
55
60
65
69.0
cm-1
%T
2926
23592340
1731
1386
1209
1171
887
794
763
763 794 cm
-1

11. Gas Chromatography Mass
Spectrophotometer
•PRINCIPLE:
•GCMS is a technique in which a complex organic
mixture gets separated and detected (identified )
by a detector (mass spectrophotometer).

12. Gas Chromatography Mass
Spectrophotometer
•What is PY GCMS ?
•GCMS is the result of technological coupling of chromatographic and spectroscopic
measuring techniques.
•Chromatography is used to separate closely related components of complex
organic mixtures.
•Mass spectrometry is a versatile and widely used tool for identifying the
compounds in the sample.
•Pyrolysis means heating the sample at a high temperature which is one of the
important techniques in the study of polymers.
•Therefore, PY-GCMS remains the most convenient way to analyze polymers.

13. Instrument Features of GCMS
Available at IRMRA:
Model: QP 5050A (Shimadzu).
Columns Available: DB1,DB5,Carbowax.
Detectors: Mass and FID.
Column Operation Temperature:20-300
0
C.
Library Available: 1.Wiley (more than 2.5
lakhs of organic compounds)
2.PYRDB ( 150 plastic samples)
Special feature: Pyrolyser (max temp.- 800
0
C

14. Testing Procedure:
•1. 25-30 gm of rubber product is extracted with acetone as per ASTM D 297.
•2. From rubber product acetone removes
Rubber resins
Free sulfur
Acetone soluble plasticizer, accelerators, and their decomposition
products ,AO,Fatty acids, processing aids, etc.
•3.This acetone extract is concentrated and a fixed quantity is injected on to the
column after selecting proper parameters like injection temperature, detector
temperature, split ratio, etc.

15. Testing Procedure
•4. This mixture gets separated on the column depending on their mol.wt.
•5. Chemicals are identified by library search.
•6. Sometimes decomposition fragments of accelerators or AO are obtained- they
are to be correlated to original accelerators or AO.
•7. Thus, qualitative and quantitative analysis are possible by GCMS.

20. OTHER APPLICATIONS OF
GCMS
Rubber and Plastic Industry: Identification
of rubbers and plastics:
•Rubber Monomer present
•Natural rubber Isoprene
•Butyl rubber Isoprene, Isobutylene
•Nitrile rubber Acrylonitrile, butadiene
•Identification of blooms.
Estimation of blend ratio of polymers.
To study the structural changes/fragmentation pattern of polymers and chemicals.