Supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) are
used to study the presence of additives in polymers that are used in living systems.
Representative samples are used to illustrate and develop the extraction capability of the
system with extracts being analysed both by on-line and off-line SFC, gas
chromatography-mass spectrometry (GC-MS), and gravimetrically. Different types of
additives are employed illustrating their chromatographic behaviour and the uses of
both flame ionisation (FID) and UV /Visible detection. The qualitative aspects of the
analysis of polymer additives are augmented by on-line linking of a mass spectrometer
(MS) to the SFC. The spectra obtained from this system are compared with other probe-MS,
GC-MS and library spectra that are available to establish the quality of the spectra
obtained. The development of on-line SFE-SFC-MS for the analysis of polymer
additives allows for a quick qualitative analysis of the compounds present in polymer
samples. Using a set of flame retardants, which are difficult to analyse by comparable
methods, on-line SFE-SFC quantitative investigations are performed on polyurethane
foams containing these compounds using short extraction times and varying pressures.
The results are compared with the Soxhlet extracts and off-line SFE-SFC analysis of the
same samples. An extraction model is used to explain the pattern of extraction of
additives from both polyurethane foams and laboratory prepared polyvinyl chloride
formulations. The studies are performed using different mobile phase strengths and
particle sizes to establish the processes involved. The extracts are analysed quantitatively
by SFC-FID and GC-FID.
A Doctoral Thesis. Submitted in partial fulfilment of the requirements for the award of Doctor of Philosophy at Loughborough University.