Title page for ETD etd-08012012-040411


Type of Document Master's Thesis
Author Turner, Kelly A.
URN etd-08012012-040411
Title Polyethylene glycol stationary phases for capillary gas chromatography
Degree Master of Science
Department Chemistry
Advisory Committee
Advisor Name Title
McNair, Harold M. Committee Chair
Mason, John G. Committee Member
Taylor, Larry T. Committee Member
Keywords
  • Capillarity
Date of Defense 1988-09-05
Availability restricted
Abstract
The chromatographic properties of various silicone stationary phases for capillary gas chromatography have been extensively studied, yet the properties of nonsilicone phases have not been so well investigated. The most popular nonsilicone phases are the high molecular weight polyethylene glycols (HMW PEG) which are commercially available in a wide range of molecular weights, cross—linkable and uncross-linkable (Carbowax 2OM and 4OM, the Superox series, etc.). Their most outstanding features are their unique polarity and selectivity; for this reason these phases are widely used in the analysis of aqueous solutions, essential oils, and perfumes.

Unfortunately HMW-PEG's are very sensitive to slight differences in preparation and handling procedures which can cause analyses to differ with each laboratory, each column, and even each use. HMW—PEG's also suffer from low temperature stability, a high minimum allowable operating temperature, and have lower diffusion coefficients than silicone phases.

This study examines the efficiency differences of eight columns differing only in immobilization procedure and added functional groups. Comparison is made using HETP versus u and separation number (TZ) versus u curves. These curves offer important information, in particular, the effect of carrier gas, u, column operating temperature, degree of cross—linking, and cross-linking temperature on chromatographic efficiency and separation number. In addition, the contributions of the CL (resistance to mass transfer in the liquid phase) and DL (diffusion coefficient in the liquid phase) terms in the Golay equation are calculated [1]. Solids at room temperature, PEG stationary phases undergo a solid-liquid phase transition within their useful temperature range. The effect of this transition on the chromatographic properties is investigated using efficiency, separation number, capacity ratio, and retention index versus temperature curves. Four more columns, in addition to the eight mentioned above, demonstrate the influence of end-groups and the molecular weight of the stationary phase on the phase transition temperature range.

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