Fourier Transform Infrared Spectroscopy Industrial Sample Analysis

Trevor Woods Polymer Research Centre School of Physics

William Herschel

Infrared Spectrum

Sample Analysis

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.

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

Types of Analysis
Chemical Analysis: Match spectra to known databases i.e. identify an unknown compound
100

95 C4 Green Contaminant 90

85 2856.93 %Transmittance 80 2923.87 75 3306.85 694.80

1271.70 70 1457.58 65

778.03 796.99

1508.25 60 1636.48 55 4000 3000 2000 Wavenumbers (cm-1) 1541.14 1000 1070.03

Unknown Green Contaminant found in production line

Spectra obtained by FTIR Analysis.

Case Study 1

Case Study 1
100 95 90 85 80 75 70 65 %Transmittance 60 55 50 45 40 35 30 25 20 15 10 4000 3000 2000 Wavenumbers (cm-1) 3301.15 1642.30 1000 2936.16 1544.66 2863.86 3074.03 POLYAMIDE 6 + POLYAMIDE 6,6 1202.95 1372.53 1265.10 1463.33 688.49 1636.48 1541.14 3306.85 1271.70 1457.58 1508.25 1070.03 694.80 778.03 796.99 2856.93 2923.87 C4 Green Contaminant

FTIR Green Contaminant Polymer Library Match. i.e. Green Contaminant Polyamide 6,6 material

Case Study 2

Brown contaminant on Moulding production line

100 98 96 94 92 90 88 86 84 %Transmittance 82 80 78 76 74 72 70 68 66 64 62 60 58 4000 3000 2000 Wavenumbers (cm-1) 1000 2926.54 1017.81 1648.88 1508.43 1543.41 1078.04 Brown Contaminant 1409.20 1153.20

Resulting FTIR analysis spectra.

Case Study 2
130 120 Brown Contaminant 110 100 1648.88 90 80 70 60 50 40 2886.33 30 1371.78 20 3421.16 10 4000 3000 2000 Wavenumbers (cm-1) 1000 1060.68 608.11 1646.94 897.93 2926.54 1153.20 1078.04 1017.81

%Transmittance

Cellulose Library Match

Brown Contaminant Library match - Cellulose contaminant

Case Study 3

3 moulding from different produciton times.. Same material?....

200 180 Acceptable 160 140 120 100 %Transmittance 80 60 40 20 New Batch Resin 0 -20 -40 -60 -80 4000 3000 2000 Wavenumbers (cm-1) 1000 Unknown Material

Case Study 3

*Acceptable OL #1267; LEXAN 141-112*POLYCARBONATE RESIN

0.8

0.6

0.4

0.2

0 4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400

Case Study 3
DB HU ID 2107 Tag HQI MAKROLON E 978.85 MAKROLON SDP 16 HU 2109 976.02 BAYBLEND T 45 MN HU 2111 972.57 MAKROLON GV 181 HU 2110 971.77 THERMOCOMP DL-4040*FILLED POLYCARBONATE RESIN MAKROLON 281 HU 2108 954.36 POLYCARBAFIL J-50/10-N (NATURAL)*10% GLASS REINFORCED POLYCARBONATE BASE RESIN POLYCARBAFIL J-50/10-N (NATURAL)*10% GLASS REINFORCED POLYCARBONATE BASE RESIN MAKROLON VERSUCHSPRODUKT KL 11140 PANLITE RESIN*POLYCARBONATE OL 1266 826.77 Name Spectrum

OL

1270

967.84

OL

1269

921.85

SR

198

921.85

HU

2113

875.82

Case Study 4 Incoming material analysis for product quality control

100 95

90

3076.59 Dowlex IP-10 ZE31019Z2B

1369.16 1641.85 1715.98 909.53 1463.23 991.54 719.68

85

80 %Transmittance

75 2849.54 70 2918.96

65

60

55

50 3000 2000 Wavenumbers (cm-1) 1000

100 95 90 85 80 75 70 65 %Transmittance 60 55 50 45 40 35 30 25 20 15 10 3000 2849.18 2917.50 2000 Wavenumbers (cm-1) 1000 1463.15 909.26 1641.41 991.66 719.80 3077.04 Dowlex IP-10 Batch No. X128019Z2D 965.39 1377.44 1415.18 2849.54 2918.96 3076.59 Dowlex IP-10 ZE31019Z2B 1641.85 1715.98 1463.23 1369.16 909.53 991.54 719.68

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

Overlay of samples

100

80

% W eig h t

60

40

20

0 0 100 200 300 400 500 600 700 800 900 1000

Temperature (deg C)

Temperature range from ambient to 1000C Scanning rates from 0.1C to 200C/min Temperature precision 2C Sample masses as little as 2mg The sample atmosphere can be either nitrogen or air

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

Contact angle

Spreading Complete wett. Partial wetting

SL= SV

Negligible wett.

Non-wett

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