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Thermogravimetric Analysis – Fourier Transform Infra-Red Spectrometry By analysing the exhaust gasses from the TGA it may be possible to identify, in part, the decomposition products produced at a given temperature. Unlike analysis of the scCO2 processed samples, the polymer decomposition samples pass through their decomposition temperatures and as such may evolve condensable vapours. Transfer between the TGA and the FT-IR gas analysis cell requires the use of a Heated Transfer Line (HTL) to prevent the condensation of considerable proportions of the evolved vapours and gasses. As the TGA utilised TGA Method 2, presented previously, emphasis will be on the FT-IR parameters. Three-dimensional FT-IR spectra were acquired over the range of 700 cm-1 – 4000 cm-1 with a resolution of 4 cm-1. Individual spectra comprised of 32 accumulations, through a 7.1 mm aperture with a scan speed of 2 mm s-1, were acquired for a period of 95 minutes to coincide with TGA Method 2. These parameters, with the exception of time, were also used to carryout a background spectrum prior to analysis of any samples. The flowrate through the HTL was approximately 200 ml min-1, with the temperature of the HTL and gas analysis cell being 353 K. Scanning Electron Microscopy and Energy Dispersive X-Ray Spectrometry Samples were imaged using a Philips XL30 FEG ESEM Scanning Electron Microscope (Philips, Netherlands) with an amplitude of 20 kV. The working distance (WD) was adjusted according to the sample under analysis as was the magnification. Where necessary the samples were cut into sections, measuring approximately 15 mm2, and loaded onto standard SEM stubs that had been coated with an adhesive film. The samples were then 124PDF Image | Supercritical Fluids and Their Application to the Recycling of High-Performance Carbon Fibre Reinforced Composite Materials
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