Fourier Transform Infrared Spectroscopy

Industrial Sample Analysis

Trevor Woods
Polymer Research Centre
School of Physics
William Herschel
Infrared Spectrum
In infrared spectroscopy, IR radiation is passed through a sample.
Some of the infrared radiation is absorbed by the sample and
some of it is passed through(transmitted).
The resulting spectrum represents the molecular absorption and transmission, creating a
molecular fingerprint of the sample
Like a fingerprint no two unique molecular structures produce the same infrared
spectrum
This makes infrared spectroscopy useful for several types of analysis.
Sample Analysis
Attentuated Total Reflectance
Sample always in contact with infrared beam
Reflectance mode FTIR beam bounced off sample
i.e. dark/rubber/carbon samples
Types of Analysis
Structural ideas: Can determine what chemical groups are in a
specific compound
Absorbance wavelength/frequency of some typical bonds
Chemical Analysis:
Match spectra to known databases
i.e. identify an unknown compound
Types of Analysis
Unknown Green Contaminant
found in production line
694.80
778.03
796.99
1070.03
1271.70
1457.58
1508.25
1541.14
1636.48
C4 Green Contaminant
2856.93
2923.87
3306.85
55
60
65
70
75
80
85
90
95
100
%
T
r
a
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s
m
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c
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1000 2000 3000 4000
Wavenumbers (cm-1)
Spectra obtained by FTIR Analysis.
Case Study 1
694.80
778.03
796.99
1070.03
1271.70
1457.58
1508.25
1541.14
1636.48
C4 Green Contaminant
2856.93
2923.87
3306.85
688.49
1202.95
1265.10
1372.53
1463.33
1544.66
1642.30
POLYAMIDE 6 + POLYAMIDE 6,6
2863.86
2936.16
3074.03
3301.15
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
%
T
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1000 2000 3000 4000
Wavenumbers (cm-1)
FTIR Green Contaminant Polymer Library Match.
i.e. Green Contaminant Polyamide 6,6 material
Case Study 1
Brown contaminant on Moulding production line
1017.81
1078.04
1153.20
1409.20
1508.43
1543.41
1648.88
Brown Contaminant
2926.54
58
60
62
64
66
68
70
72
74
76
78
80
82
84
86
88
90
92
94
96
98
100
%
T
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s
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t
a
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c
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1000 2000 3000 4000
Wavenumbers (cm-1)
Resulting FTIR analysis spectra.
Case Study 2
1017.81
1078.04
1153.20
1648.88
Brown Contaminant
2926.54
608.11
897.93
1060.68
1371.78
1646.94
Cellulose Library Match
2886.33
3421.16
10
20
30
40
50
60
70
80
90
100
110
120
130
%
T
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1000 2000 3000 4000
Wavenumbers (cm-1)
Brown Contaminant Library match - Cellulose contaminant
Case Study 2
Acceptable
Unknown Material
New Batch Resin
-80
-60
-40
-20
0
20
40
60
80
100
120
140
160
180
200
%
T
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1000 2000 3000 4000
Wavenumbers (cm-1)
Case Study 3
3 moulding from different
produciton times..
Same material?....
4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400
0
0.2
0.4
0.6
0.8
1
*Acceptable
OL #1267; LEXAN 141-112*POLYCARBONATE RESIN
Case Study 3
DB ID Tag HQI Name Spectrum
HU 2107 978.85
MAKROLON E
HU 2109 976.02
MAKROLON SDP 16
HU 2111 972.57
BAYBLEND T 45 MN
HU 2110 971.77
MAKROLON GV 181
OL 1270 967.84
THERMOCOMP DL-4040*FILLED
POLYCARBONATE RESIN
HU 2108 954.36
MAKROLON 281
OL 1269 921.85
POLYCARBAFIL J-50/10-N
(NATURAL)*10% GLASS REINFORCED
POLYCARBONATE BASE RESIN
SR 198 921.85
POLYCARBAFIL J-50/10-N
(NATURAL)*10% GLASS REINFORCED
POLYCARBONATE BASE RESIN
HU 2113 875.82
MAKROLON VERSUCHSPRODUKT KL 1-
1140
OL 1266 826.77
PANLITE RESIN*POLYCARBONATE
Case Study 3
719.68
909.53
991.54
1369.16
1463.23
1641.85
1715.98
Dowlex IP-10 ZE31019Z2B
2849.54
2918.96
3076.59
50
55
60
65
70
75
80
85
90
95
100
%
T
r
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s
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1000 2000 3000
Wavenumbers (cm-1)
Case Study 4
Incoming material analysis for product quality control
719.68
909.53
991.54
1369.16
1463.23
1641.85
1715.98
Dowlex IP-10 ZE31019Z2B
2849.54
2918.96
3076.59
719.80
909.26
965.39
991.66
1377.44
1415.18
1463.15
1641.41
Dowlex IP-10 Batch No. X128019Z2D
2849.18
2917.50
3077.04
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
%
T
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1000 2000 3000
Wavenumbers (cm-1)
Incoming raw material matched to previously used production sample
Raw material analysed kept in storage for future analysis
Material monitoring system ensures customer/supplier satisfaction.
TGA Analysis of Polymer Materials
Investigate trapped solvent issues
%filler issues
Thermal stability issues
Temperature range fromambient to 1000C
Scanning rates from0.1C to 200C/min
Temperature precision 2C
Sample masses as little as 2mg
The sample atmosphere can be either nitrogen or air
Overlay of samples
0
20
40
60
80
100
0 100 200 300 400 500 600 700 800 900 1000
Temperature (deg C)
%

W
e
i
g
h
t
DSC Analysis of Polymer Materials.
Temperature range from 100 to 500C
Scanning rates from 0.01 to 200C/min
Polymer comparison
Crystallisation, glass (Tg) and melt transitions (Tm)
processing procedures which may affect the
performance of the finished product
Degradation during transport, storage or handling
GPC Analysis of Polymer Materials.
Determine the average molecular weight
and the molecular weight distributions of
polymers
Determine the polydispersity and degree of
polymerisation of a polymer
Determine whether degradation has
occurred within the polymer
Dynamic Mechanical Analysis
Dynamic Mechanical Analysis is a technique that measures
the modulus (stiffness) and damping (energy dissipation)
of materials as they are deformed under periodic stress.
Polymeric materials, which are viscoelastic in nature, are
subject to time, frequency and temperature effects on
mechanical properties which can be analysed by this
method
-150C 400C and a range of frequencies, 0.1Hz to 10Hz
Spreading Complete wett. Partial wetting
SL
=
SV
Negligible wett. Non-wett
Contact angle
Dynamic and Static contact angle
techniques
Determine the wettability, adhesion and
surface energy of a surface, coating or bulk
material
Measuring the effects of plasma treatment,
thin film deposits, contamination of
surfaces
Polymer Analysis:
Contact :
Trevor Woods woodst@tcd.ie
Colin Reid creid@tcd.ie