Quantitative Analysis of Additives in Low Density Polyethylene Using On-line Supercritical Fluid Extraction /Supercritical Fluid Chromatography
Lucy Ying Zhou
Thesis submitted to the Faculty of the Virginia Polytechnic Institute and State University in partial fulfillment of the requirements for the degree of
Master of Science in Chemistry
Larry T. Taylor, Chair Harry Dorn Harold M. McNair
June 1998 Blacksburg, Virginia
Keywords: Supercritical, Extraction, Chromatography, On-line, Polymer additives, HPLC
Copyright 1998, Lucy Y. Zhou
Quantitative Analysis of Additives in Low Density Polyethylene Using On-line Supercritical Fluid Extraction /Supercritical Fluid Chromatography Lucy Ying Zhou (ABSTRACT)
Polymer additives exemplify many classes of compounds which possess a wide variety of chemical (i.e., phenols, amides, esters) and physical (i.e., volatility, solubility) properties. They are incorporated into polyolefins and other such polymeric materials for a number reasons: (a) to prevent degradation by ultraviolet light, heat, and oxygen; (b) to aid in the processing of the polymer; and (c) to modify the physical properties of the polymer. Since the purity and amount of additive can affect polymer properties, it is very important to characterize and quantify additives in polymer products. Traditional liquid solvent/polymer extraction methods, which involve dissolution/precipitation, are timeconsuming, uneconomical, and the recoveries are significantly lower than 90%. In recent years, analysis with supercritical fluids (SFs) has emerged as an alternative analytical technique because SFs afford higher diffusivity and lower viscosity. In this research, an on-line Supercritical Fluid Extraction (SFE)/Supercritical Fluid Chromatography (SFC) system was assembled to provide efficient extraction and separation of polymer additives with quantitative results. The effects of various SFE/SFC parameters, such as trapping temperature, injection temperature, extraction pressure and temperature, dynamic extraction time, and fluid flow rate on extraction and separation efficiencies of different additive standards (i.e., BHT, BHEB, Isonox 129, Irganox 1076 and Irganox 1010) were investigated. Optimized conditions were employed to quantitatively extract additives from LDPE. Identification of additives was performed by comparing the retention time with each additive standard. Results obtained from on-line SFE/SFC were compared to results from off-line SFE/High Performance Liquid Chromatography (HPLC) and off-line Enhanced Solvent Extraction (ESE)/HPLC.

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