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Lecture 49

Apr 14, 2025

Lecture on Gas Chromatography: Gas-Solid vs. Gas-Liquid

Overview

  • Discussed Gas Chromatography (GC) focused on Gas-Liquid Chromatography (GLC) and now shifting to Gas-Solid Chromatography (GSC).

Gas-Solid Chromatography (GSC)

  • Basis: Adsorption of gaseous molecules on a solid surface.
  • Distribution Coefficients (K): Higher in GSC than in GLC, leading to greater separation efficiency.
  • Applications:
    • Useful for components not retained by GLC, including:
      • Air components, Hydrogen sulfide, Carbon disulfide, Nitrogen oxides, Carbon monoxide, Carbon dioxide, and rare gases.
  • Columns Used:
    • Both packed and open tubular columns.
    • Open tubular columns have a thin layer of adsorbent on the inner wall.

Types of Adsorbents

  1. **Molecular Sieves:"
    • Composed of aluminum silicate ion exchangers.
    • Molecules as small balls, facilitating ion exchange between mobile and stationary phases.
    • Pore sizes depend on present cation: Typically 4, 5, 10, or 13 angstroms.
    • Smaller molecules penetrate particles' interior for adsorption.
  2. Porous Polymers:
    • Made from styrene cross-linked with divinyl benzene.
    • Uniform pore size controlled by cross-linking.
    • Useful for separating gaseous polar species such as Hydrogen sulfide, Nitrogen oxides, Water, Carbon dioxide, Methanol, and Vinyl chloride.**

Example Spectrum and Separation Techniques

  • Columns Compared:
    • 5 x 1/8 micro molecular sieve column vs. plot column.
  • Gas Liquid Column:
    • Retains only Carbon dioxide (CO2), other gases pass through.
    • CO2 is identified as 'b' in exhaust mixtures.
    • Need to avoid permanent absorption of CO2 on sieves by switching direct flow upon CO2 elution.
    • Involves coordination between ordinary gas-liquid column and molecular sieve column.

Column Operation

  • Switching Mechanism:
    • When CO2 elutes, the flow is switched to avoid absorption.
    • After CO2 signal returns to zero, flow switches back to separate and evolve remaining sample components.
    • Coordination helps prevent CO2 retention on sieves and prolong column utility.

Plot Column Application

  • Open Tubular Column:
    • Lined with porous polymer.
    • Demonstrates effective separation using the plot column.

These notes provide an overview of Gas-Solid Chromatography, focusing on its principles, adsorbents, applications, and practical column operations.