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    Chapter

    Introductory Chapter: Gas


    Chromatography - The Most
    Versatile Analytical Technique
    Peter Kusch

    1. Definition and short history of gas chromatography

    Gas chromatography (GC) is a type of chromatography. According to the


    International Union of Pure and Applied Chemistry (IUPAC) recommendation, gas
    chromatography is defined as a separation technique in which the mobile phase is
    a gas. Gas chromatography is always carried out in a column [1]. GC is a separation
    and detection method for sample mixtures, whose components can be volatilized
    without thermal decomposition. The analytical procedure is used for the determi-
    nation of organic substances; usually molecules have a molecular mass of less than
    500 g/mol and a boiling point of less than 400°C. GC is a technique used to separate
    mixtures of gaseous chemical compounds based on differences in the compounds’
    relative affinities for a solid (gas-solid chromatography) or liquid (gas-liquid
    chromatography) stationary phase held within a column.
    Gas-liquid partition chromatography was invented by Martin and James from
    the National Institute for Medical Research, London, in 1952. The invention of
    this technique is generally attributed to the inventors in their 1952 published
    paper in the Biochemical Journal [2]. In this publication the theory of the partition
    column has been extended to cover a compressible mobile phase, and gas-liquid
    partition columns were described for the separation of volatile fatty acids. In
    the same year, the Nobel Prize in chemistry was awarded jointly to Martin and
    Synge for their invention of partition chromatography. Starting from this time, gas
    chromatography has become one of the most important and widely applied ana-
    lytical techniques in modern chemistry. The first commercial gas chromatograph
    was introduced in 1955 by Perkin-Elmer (USA). Subsequently, this method was
    used to study petrochemical products. Today, gas chromatography is one of the
    most widespread investigation methods of instrumental analysis. This technique
    is used in the laboratories of the chemical, petrochemical, and pharmaceutical
    industries, in the research institutes and also in the clinical and environmental
    and food and beverage analyses. Recent developments in GC have resulted in the
    introduction of better and selective fused silica capillary columns and methods
    for sample preparation. Newer separation and detection solutions, such as fast
    GC, multidimensional separation GC techniques (GC × GC), and hyphenation
    of GC and GC × GC with mass spectrometry (MS), with triple quadrupole mass
    spectrometry and with time-of-flight mass spectrometry (TOF-MS), have been
    developed and become industrial routine. Analytical pyrolysis (Py) technique
    hyphenated to GC and GC/MS has extended the range of possible tools for the
    characterization of synthetic polymers and copolymers. This technique has been

    1
    Gas Chromatography - Derivatization, Sample Preparation, Application

    used extensively over the last 30 years as a complementary analytical tool used to
    characterize the structure of synthetic organic polymers and copolymers, poly-
    mer blends, biopolymers, and natural resins [3].

    2. Multidimensional gas chromatography

    Developed by Phillips and coworker at the Southern Illinois University (USA)


    in the early 1990s, comprehensive multidimensional GC (GC × GC or 2D GC) is
    a powerful technique for samples containing very large numbers of compounds
    of interest and also for samples which exhibit high chemical complexity. This
    technique can be used to separate very complex mixtures, such as those found in
    the petrochemical, environmental, and food and fragrance industries [4–6]. The
    method uses two capillary columns, typically of very different polarities, installed
    in series with a modulator in between. The first column is in principle nonpolar
    or low polar, and the second column is polar. The length of the first column might
    typically be 20–30 m, the inner diameter 0.25 mm, and the film thickness 0.25 μm.
    The second column is typically shorter (1–2 m), the inner diameter is narrower
    (0.1 mm), and the stationary phase is thinner (0.1 μm), to allow for faster separa-
    tions. The entire assembly is located inside the GC oven [6]. The modulator collects
    effluent from the first column for a fraction of the time equal to peak width. The
    modulator focuses the material collected from each cut into a very narrow band
    through flow compression. It introduces the bands sequentially onto the second
    column, resulting in additional separation for each band injected onto the second
    column [4–9]. The most common data transformation is the construction of a 2D
    representation, in which one axis represents the separation on the first column (first
    dimension), and the other axis represents the secondary column separation (second
    dimension). Therefore, the look of GC × GC chromatograms appears completely
    different from conventional GC chromatogram showing a two-dimensional plane
    where analyte spots are scattered about [7, 8]. A contour plot, using elevation lines
    or color coding, represents the signal intensity. 2D GC data are primarily used for

    Figure 1.
    2D GC plot of a refinery stream boiling at diesel temperature range. The scale indicates the relative signal
    intensity. Figure reprinted from Ref. [10] with permission from ACS.

    2
    Introductory Chapter: Gas Chromatography - The Most Versatile Analytical Technique
    DOI: http://dx.doi.org/10.5772/intechopen.81693

    qualitative analysis; however, quantitative multidimensional GC analysis is also


    possible [9]. Figure 1 shows an exemplary 2D GC plot of a refinery stream boiling at
    diesel temperature range [10].
    In this book, state of the art of gas chromatography and new developments and
    applications are presented. New sample preparation techniques, derivatization
    methods, and hyphenation with mass spectrometry are described.

    Author details

    Peter Kusch
    Department of Applied Natural Sciences, Bonn-Rhein-Sieg University of Applied
    Sciences, Rheinbach, Germany

    *Address all correspondence to: [email protected]

    © 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms
    of the Creative Commons Attribution License (http://creativecommons.org/licenses/
    by/3.0), which permits unrestricted use, distribution, and reproduction in any medium,
    provided the original work is properly cited.

    3
    Gas Chromatography - Derivatization, Sample Preparation, Application

    References

    [1] IUPAC Compendium of Chemical


    Terminology, International Union of
    Pure and Applied Chemistry, Version
    2.3.3. 2014

    [2] James AT, Martin AJP. Gas-liquid


    partition chromatography: The
    separation and micro-estimation of
    volatile fatty acids from formic acid
    to dodecanoic acid. The Biochemical
    Journal. 1952;50(5):679-690

    [3] Kusch P. Pyrolysis—Gas


    Chromatography/Mass Spectrometry
    of Polymeric Materials. London, UK:
    World Scientific Europe; 2018

    [4] Liu Z, Phillips JB. Comprehensive


    two-dimensional gas chromatography
    using an on column thermal modulator
    interface. Journal of Chromatographic
    Science. 1991;29(6):227-231

    [5] Phillips JB, Xu J. Comprehensive


    multi-dimensional gas chromatography.
    Journal of Chromatography A.
    1995;703:327-334

    [6] Comprehensive GC System Based


    on Flow Modulation for the 7890A GC,
    Application Brief. Wilmington, DE,
    USA: Agilent Technologies; 2008

    [7] Hinshaw JV. Comprehensive two-


    dimensional gas chromatography. LCGC
    Europe. 2004;17(2):86-95

    [8] Mondello L. GC  × GC Handbook,


    Fundamental Principles of
    Comprehensive 2D GC. Japan:
    Shimadzu; 2012

    [9] Taylor T.  A short introduction to


    multidimensional GC. LCGC North
    America. 2012;30(9):870

    [10] Wang FC, Qiang K, Green


    LA. GCxMS of diesel: A
    two-dimensional separation
    approach. Analytical Chemistry.
    2005;77(9):2777-2785

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