Quantitation of the amount of finish applied during fiber manufacturing is an important industrial quality control process. Finish levels that are too low result in excessive fiber and mechanical wear. On the other hand, overly high finish levels may cause residue buildup on the processing equipment. Removal of the finish has traditionally been done with solvents such as chloroform or Freon followed by gravimetric or spectroscopic analysis of the removed material. Quantitation of low molecular weight oligomeric material is another important quality control practice for the fiber industry in that the presence of these species and their concentration affect the physical properties of the polymer. Also, excessively high concentrations of oligomers may result in residue deposits on processing equipment. Typical conventional methods for determining the concentration of oligomers present in fibers involve large quantities of organic solvent for removal of the oligomers followed by chromatographic analysis. Increased government regulation of chlorinated and other solvents has led to investigations of alternate methods of extraction. Several studies have shown that supercritical fluid extraction (SFE) using carbon dioxide as the extraction fluid is an important alternative to conventional organic solvent extraction for the removal of both textile finishes and oligomeric material. This research seeks to extend the previous studies regarding the application of SFE for the quantitation of finish and oligomers from nylon 6,6 fibers. The effects of pressure, extraction temperature, modifier percentage, static extraction time, and dynamic extraction time on the supercritical fluid extraction efficiency of nylon 6,6 oligomers were examined. Results from the SFE methods for both finish and oligomer extractions were compared to results from conventional solvent extraction. The extracted oligomers were identified by HPLC with coupled on-line atmospheric pressure chemical ionization mass spectrometry (APCI-MS) and HPLC fractionation coupled with off-line Liquid Secondary Ion Mass Spectrometry (LSIMS). / Master of Science