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 n s m i t t a n c e 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 r a n s m i t t a n c e 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 r a n s m i t t a n c e 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 r a n s m i t t a n c e 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 r a n s m i t t a n c e 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 a n s m i t t a n c e 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 r a n s m i t t a n c e 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