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DSM
Polymer troubleshooting and QC with FTIR
DSM Research, CT&A - Analytical Services
December 2002
Peter Meijers
Analytical Services
P. Meijers
DSM Research
Research
DSM
Polymer troubleshooting and QC with FTIR
Topics to be covered today
- Where do we analyse?
- Why do we analyse?
- What do we analyse?
- How do we analyse?
- For whom do we analyse?
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Polymer troubleshooting and QC with FTIR
Research Campus Geleen
Life
Sciences
Industrial
Chemicals
Performance
polymers
SABIC
Petrochemical
Europe
Center for Technology & Analysis
Technology 60
DSM R&D outside
Campus Geleen
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Anal. Services 70 FTE
Third parties
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Polymer troubleshooting and QC with FTIR
Analytical Services (70 FTE)
Additive analysis
In process analysis
Elemental analysis
Microscopy
Thermal analysis
Mathematics & statistics
Optical Spectroscopy
Nuclear Magnetic Resonance
Molecular characterisation
Chromatogr. & mass spectrom.
Engineering plastics, functional groups & titrimetry
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Polymer troubleshooting and QC with FTIR
Optical spectroscopy (6 FTE)
- Raman spectroscopy
- UV-VIS spectroscopy
- Colorimetry
- FT IR spectroscopy
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Polymer troubleshooting and QC with FTIR
FT-IR spectroscopy (MID-IR 4000 – 400 cm-1):
- Transmission
- Transmission via microscope
- Reflection (ATR crystals: Diamond, Germanium, Silicon)
- Multi bounce HATR (Zinc Selenide)
- Real-time kinetic analysis
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Polymer troubleshooting and QC with FTIR
Some examples of Quality Control with FTIR
PE:
Branching level, type of comonomer
C=C unsaturation: end, side, trans
MAA-content in PE-MAA
PP:
C2 and stabilizer content
EPDM:
C2/C3 ratio (ASTM D3900) and diene content (D6047)
Stabilizer content
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Polymer troubleshooting and QC with FTIR
C2/C3 ratio in EP(D)M according to ASTM D3900
1 ,00 0
C2
0 ,95
0 ,90
0 ,85
720,93
0 ,80
peak height = 0,8532 A
0 ,75
0 ,70
0 ,65
peak ratio C3 height / C2 height is a measure for C2 content
0 ,60
0 ,55
A
0 ,50
0 ,45
0 ,40
peak height = 0,0893 A
1154,73
0 ,35
0 ,30
C3
0 ,25
0 ,20
0 ,15
0 ,10 0
1 25 0,0
1 20 0
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1 15 0
1 10 0
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1 05 0
1 00 0
9 50
cm-1
9 00
8 50
8 00
7 50
7 00
6 50 ,0
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Polymer troubleshooting and QC with FTIR
Troubleshooting with FTIR
1. Identification
2. Complaints
3. Competitor analysis
4. Research for third parties
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Polymer troubleshooting and QC with FTIR
1. FTIR identification
Unknown sample
organic
NMR
Microscopy
PyGC
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FTIR
inorganic
XRF
Microscopy
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Polymer troubleshooting and QC with FTIR
Examples of FTIR spectra of inorganics
talc
chalk
1 00 ,0
1 00 ,1
95
98
90
85
96
80
94
75
2511,70
3676,60
1794,96
92
70
712,76
90
65
88
60
86
55
%T
%T
50
84
45
82
40
80
35
78
993,35
30
76
25
668,01
20
15
72
1 0,0
7 0,0
4 00 0,0
3 60 0
3 20 0
2 80 0
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2 40 0
2 00 0
1 80 0
cm-1
1 60 0
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1 40 0
1 20 0
1 00 0
8 00
6 50 ,0
873,53
74
4 00 0,0
1413,61
3 60 0
3 20 0
2 80 0
2 40 0
2 00 0
1 80 0
cm-1
1 60 0
1 40 0
1 20 0
1 00 0
8 00
6 50 ,0
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Polymer troubleshooting and QC with FTIR
2. FTIR complaints
- Blooming
- Small contaminations (up to 10 µm)
Organic: cellulose, gels, PE wax, SBR, Ca/Zn-stearate, teflon
Inorganic: calcium carbonate, calcium oxide, clay, mica, talc
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Polymer troubleshooting and QC with FTIR
Example of complaint: SBR gel in EPDM compound
3 0,0
28
26
24
22
20
18
16
%T
14
12
10
3061,21
1493,30
8
1376,17
965,98
6
910,83
4
699,78
2 ,0
4 00 0,0
3 60 0
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3 20 0
2 80 0
2 40 0
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2 00 0
1 80 0
cm-1
1 60 0
1 40 0
1 20 0
1 00 0
8 00
6 50 ,0
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Polymer troubleshooting and QC with FTIR
FTIR spectrum of cellulose
9 0,0
85
80
75
70
65
60
55
50
%T
45
40
35
30
25
20
15
1 0,0
4 00 0,0
3 60 0
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3 20 0
2 80 0
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2 40 0
2 00 0
1 80 0
cm-1
1 60 0
1 40 0
1 20 0
1 00 0
8 00
6 50 ,0
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Polymer troubleshooting and QC with FTIR
FTIR spectrum of polypropylene
9 5,0
90
85
80
75
70
807,91
65
%T
60
55
1451,77
2838,05
50
1375,54
2949,50
45
40
2917,45
3 5,0
4 00 0,0
3 60 0
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3 20 0
2 80 0
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2 40 0
2 00 0
1 80 0
cm-1
1 60 0
1 40 0
1 20 0
1 00 0
8 00
6 50 ,0
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Polymer troubleshooting and QC with FTIR
3. FTIR competitor analysis
Compound composition:
- polymer type
- filler type (chalk, clay, talc)
(via TG: amount of polymer, carbon black, ash rest)
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Polymer troubleshooting and QC with FTIR
4. (FTIR) Research for third parties
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Polymer troubleshooting and QC with FTIR
FTIR = A POWERFUL TOOL
- Direct measurement on material
- Quick method
- Much chemical info
- Not destructive
- Small amounts of sample needed
However: it is NOT absolute (reference method is needed for
quantification)
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Polymer troubleshooting and QC with FTIR
The Analytical service group at Research campus Geleen has:
- Broad toolbox
- Long history in material science
- Strong knowledge position on polymer materials
- Proprietary data bases (additives, spectra)
- Experienced and skillful people
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www.dsm-solutions.com 31(0)46 4760404
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