Emerging Techniques; Hyphenated Technologies for Polymer and Biofuel Application

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1 Emerging Techniques; Hyphenated Technologies for Polymer and Biofuel Application Scott Fraser (PhD) National Product Specialist Thermal & Elemental Analysis PerkinElmer

2 Hyphenation Possibilities Modification of Sample Environment Tracks physical changes in the sample by adjusting the environmental conditions Thermal UV DSC-UV, STA-UV Mechanical-UV/Humidity DMA-UV DMA-Humidity Can give an accurate representation of materials under given conditions representative of storage, processing, different markets etc. Evolved Gas Analysis Evolved Gas Analysis refers to measurements made on gases released from a sample being tested by a thermal analyzer. Can determine water content in food stocks/pharmaceuticals, presence of volatiles, contaminants, breakdown products etc. 2

3 3 Evolved Gas Analysis

4 Why Hyphenate? Because sometimes it s not enough to know when something happened; need to know what it was as well. TGA Mass was lost FTIR Contains gases with certain functional groups present vs. time (temperature) GCMS What were those gases 4 Complete picture in real time

5 Evolved Gas Analysis: TGA as a Source Gas is evolved in the TGA Formed in different ways either volatilization, pyrolysis, combustion, reactions etc. Data here is Mass Loss vs. Temperature or time Can determine the number of weight loss events and then monitor the off gases in secondary analysis system Quantitative for the amount of gas produced Often a complex mixture of gases 5

6 Evolved Gas Analysis: FTIR as a Secondary Analysis FTIR provides information on gases functional groups Solvent levels Detection of pseudo-polymorphs and hydrates Detection of degradation/reaction products Reaction mechanism insights 6

7 Evolved Gas Analysis: GCMS/MS as a Secondary/Tertiary Analysis Tells us what came off in a thermal event giving insight into: reaction mechanism reaction by-products which solvents are present understanding of the decomposition process Residual solvent at low levels for validation of loss on drying. Contaminants at low levels Identification of solvates obtained in crystallization process Forensic concerns on combustion Can run units in stand alone mode Higher mass range, soft ionization, and chemical ionization with oxygen resistant filament in the MS 7

8 The Transfer Line The mass flow controller and filtering system provides a Constant Gas Flow through the system. Therefore Constant Gas Pressure and Constant Gas Speed are guaranteed. The Transfer Line guarantees Constant Gas Temperature Zero mass principle ensures minimal turbulence and residue formation in line Temperature range up to 350 C Simple operation; digitally controlled 8

9 9 Polymer Safety Case Study: Polycarbonate and EVA

10 TGA Results EVA 2 Mass Loss Events 2 nd event seems complex most likely a gas mixture Polycarbonate 1 Mass Loss Event Highly reproducible 10

11 %T TGA + FTIR Results Wavenumber Name Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra Coadded Spectrum at C (Temperature based Extra 11

12 GCMS Results Elution Time (min) Likely Compound 2.42 Benzene 2.87 Toluene 3.55 Ethyl-Benzene 3.65 p-xylene 3.84 Styrene methylethyl-Benzene 4.66 Phenol 4.81 Alpha-Methyl Styrene 5.89 p-cresol ethyl Phenol propyl Phenol 8.90 m-tert-butyl, Phenol p-isopropenyl-phenol ,3 dihydro, 2-methyl Benzofuran Hexadecane, 12

13 13 Biopolymer Case Study; Recycling and Biowaste

14 Weight Remaining (%) TGA Thermogram for Biowaste Sample Thermogram Derivative Temperature ( C) 14

15 Weight Remaining (%) EGA Event # Temperature ( C) 15

16 Weight Remaining (%) EGA Event # Temperature ( C) 16

17 Weight Remaining (%) EGA Event # Temperature ( C) 17

18 Conclusions Hyphenation opens up the possibility for obtaining more information on a single sample Complex samples can also be deconvaluted, and different breakdown conditions can be examined Forensically, samples with little known information can be categorized or even deduced utilizing hyphenated technology 18

19 Thankyou For Your Attention Scott Fraser PhD National Product Specialist Thermal & Elemental Analysis PerkinElmer For the Better Level 2, Building 5, Brandon Office Business Park, Springvale Rd, Glen Waverley Australia 3150 (Ph): (Mobile): PerkinElmer