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    Chapter 27: Gas Chromatography: - Principles - Instrumentation - Detectors

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    Nihad S Zain
    This document provides an overview of gas chromatography-mass spectrometry (GC-MS). It discusses the basic principles and instrumentation of GC-MS, including common types of mass spectrometers used. It describes the three main modes of operation for GC-MS and highlights some applications like GC-FTIR. The document also covers GC columns and stationary phases, from packed columns to open tubular and capillary columns. It discusses the coating and bonding of stationary phases as well as factors that influence retention times.

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    Chapter 27: Gas Chromatography: - Principles - Instrumentation - Detectors

    Uploaded by

    Nihad S Zain
    71 views26 pages
    This document provides an overview of gas chromatography-mass spectrometry (GC-MS). It discusses the basic principles and instrumentation of GC-MS, including common types of mass spectrometers used. It describes the three main modes of operation for GC-MS and highlights some applications like GC-FTIR. The document also covers GC columns and stationary phases, from packed columns to open tubular and capillary columns. It discusses the coating and bonding of stationary phases as well as factors that influence retention times.

    Original Description:

    gas chromotography

    Original Title

    Instrumental Lecture 17

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    This document provides an overview of gas chromatography-mass spectrometry (GC-MS). It discusses the basic principles and instrumentation of GC-MS, including common types of mass spectrometers used. It describes the three main modes of operation for GC-MS and highlights some applications like GC-FTIR. The document also covers GC columns and stationary phases, from packed columns to open tubular and capillary columns. It discusses the coating and bonding of stationary phases as well as factors that influence retention times.

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    71 views26 pages

    Chapter 27: Gas Chromatography: - Principles - Instrumentation - Detectors

    Uploaded by

    Nihad S Zain
    This document provides an overview of gas chromatography-mass spectrometry (GC-MS). It discusses the basic principles and instrumentation of GC-MS, including common types of mass spectrometers used. It describes the three main modes of operation for GC-MS and highlights some applications like GC-FTIR. The document also covers GC columns and stationary phases, from packed columns to open tubular and capillary columns. It discusses the coating and bonding of stationary phases as well as factors that influence retention times.

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    Chapter 27: Gas Chromatography

    Principles
    Instrumentation
    Detectors
    Columns and Stationary Phases
    Applications

    GC-MS Schematic
    Interface less critical for capillary columns

    Several types of Mass Specs available


    - Rarely magnetic sector or time of flight
    - Usually quadrapole or ion trap for GC-MS
    - Less expensive
    - Less maintenance
    - Easy to use
    - Normally use electron multiplier as detector
    - All MS systems need ion source, either
    electron impact or chemical ionization

    Ion trap uses radio


    frequency to trap
    ions, hold or
    store them, then
    ejects them to
    detector

    Three modes of operation for GC-MS


    1) Spectral mode look at mass spectrum
    every second or so during chromatogram
    - gives most information for research or
    method development
    2) Total ion current sum signal for all ions
    as one large signal highest sensitivity
    3) Selective ion monitoring look at certain
    mass/charge ratios for compounds of
    interest routine analysis

    GC-FTIR
    - Powerful technique for identifying compounds
    - Use heated light pipe 1 to 3 mm dia

    GC-FTIR
    - Powerful technique for identifying compounds
    - Use heated light pipe 1 to 3 mm dia and 10
    to 40 cm long
    - Heat to prevent condensation of sample
    - Cool detector for sensitivity
    - Gives structural information from spectrum
    - Not very common

    GC Columns & Stationary Phases


    - Historically used packed columns
    - Stationary phase coated as a thin
    film on a high surface area solid support
    - Theoretical studies showed that unpacked
    columns with narrow diameters were better
    - Open tubular columns first developed
    - Capillary columns came later because
    - Very fragile, difficult to construct, hard to
    connect to GCs, small samples hard to detect,
    difficult to coat column walls, etc.

    Packed Columns
    - Tubing of metal, glass, Teflon, etc.
    - 2 to 3 m long and 2 to 4 mm in dia
    - Packed with diatomaceous earth (SiO2), clay,
    carbon particles, glass microbeads, polymer
    - Diameter 150-250 m (60-100 mesh) 1 m2/g
    - Thin coating of liquid stationary phase
    - Can dissolve liquid in solvent, mix with support &
    evaporate solvent
    - Very tricky to do correctly
    - Condition column at 5 oC above operating temp

    Stationary Phase Coating


    good
    bad
    Silica
    Particle

    Silica
    Particle

    Dont want stationary phase liquid coating to bleed


    or puddle in column gives zone broadening &
    poor resolution

    Open Tubular Columns  Capillary Columns


    Column evolution
    Three types
    Wall Coated Open Tubular (WCOT) open
    tube with coating on wall duh
    Support Coated Open Tubular (SCOT)
    open tube with particles of support material
    stuck to the walls
    Fused Silica Open Tubular (FSOT) WCOT
    made of fused silica

    Surface chemistry glass & silica


    are SiO2 with -OH at surface
    OH OH OH OH
    -SiOSiOSiOSiOO
    O
    O
    O
    -SiOSiOSiOSiO-

    Silanol
    group
    Silica
    core

    OH is a problem because it can adsorb polar


    substances with strong affinity causing
    peak tailing must deactivate by reacting

    React Si-OH groups with silane

    Sometimes still have OH groups


    If silica not pure may have metal impurities M-OH
    typically use high purity silica acid wash
    Same chemistry to making specialty bonded phase

    Liquid coatings on stationary


    phase should exhibit:
    1) Chemical inertness
    2) Low volatility (b.p. 100 oC > max temp)
    3) Thermal stability
    4) Good solvent characteristics (i.e. k &
    suitable)
    Many different liquid coatings have been
    used or attempted for GC, only about 10
    have withstood the test of time

    Retention time of a solute depends on K


    (partition coefficient) which is dependent on
    stationary phase must have different Ks for
    different analytes
    However, if Ks too large  long retention time
    if Ks too small  short retention time
    resulting in incomplete separation
    In choosing a stationary phase use general
    principles such as like dissolves like, polar
    groups interact with polar groups, non polar
    with non polar, etc.

    Polar groups include CN, CO, OH


    Polar analytes include alcohols, acids, amines
    Non polar  hydrocarbons
    Where analyte & stationary phase match is
    good  elution order is determined by
    boiling points

    Bonded Stationary Phases


    Use silylation chemistry to
    covalently attach stationary
    phase to solid support or column wall

    Bonded Stationary Phases


    Advantages
    - monolayer coverage can be obtained
    - reduced bleeding of stationary phase
    - longer lasting
    - better stability
    - can be solvent washed
    Chiral Stationary Phases separating stereoisomers is the ultimate in chromatography,
    separate molecules that are mirror images

    Predicting retention
    I) Selectivity Factors

    If B is a standard compound & we know , can


    then be able to identify compound A even if we
    change the the chromatographic conditions
    or go to another chromatograph, etc.
    This is limited to specific applications where a
    database is available, not universally applicable

    II) Retention Index (I)


    Proposed by Kovats in 1968
    Index based on normal alkanes
    If have a mixture of 2 known alkanes & 1
    unknown compound & the 2 knowns
    bracket unknown in tR can then
    determine I for unknown & identify it
    I = 100 x # of carbon atoms
    Regardless of column packing, temp. or
    other conditions

    Kovats Retention Index


    Doesnt work as well for other types
    of compounds (Hc), but useful in
    some cases e.g. homologous series
    Plot log adjusted retention time (tR = tR tM)
    vs number of carbon atoms is linear
    Useful in particular fields petroleum
    industry, cosmetics, pharmaceuticals, etc.
    since have their own unique standards

    Note number of
    carbons that
    would be
    calculated for
    these 3
    compounds
    based on I

    Chapter 28: High-Performance


    Liquid Chromatography (HPLC)
    Scope
    Instrumentation eluants, injectors, columns
    Modes of HPLC
    Partition chromatography
    Adsorption chromatography
    Ion chromatography
    Size exclusion chromatography

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