By : Majid Baradan Supervisid By : prof.

Ashok Shakaya

Gas Chromatography
 In gas chromatography (GC), the sample is vaporized and injected onto the head of a chromatographic column. Elution is brought about by the flow of an inert gaseous mobile phase.  The mobile phase does not interact with molecule of the analyte; its only function is to transport the analyte through the column.  Gas-liquid chromatography is based upon the partition of the analyte between a gaseous mobile phase and a liquid phase immobilized on the surface of an inert solid.

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and hydrogen. Associated with the gas supply are pressure regulators. include helium. In addition. the carrier gas system often contains a molecular sieve to remove water or other impurities. gauges. and flow meters.INSTRUMENTS FOR GC Carrier Gas-Supply Carrier gases. nitrogen. which must be chemically inert. .

.  The most common method of sample injection involves the use of microsyringe to inject a liquid or gaseous sample through a self-sealing.Sample Injection System  Column efficiency requires that the sample be of suitable size and be introduced as a “plug” of vapor. silicone-rubber diaphragm or septum into a flash vaporizer port located at the head of the column (the sample port is ordinarily about 50oC above the boiling point of the least volatile component of the sample). slow injection of oversized samples causes band spreading and poor resolution.

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5% to 2% relative.  The sampling loop is filled by injection of an excess of sample. .Sample Injection System  For quantitative work. more reproducible sample sizes for both liquids and gases are obtained by means of a rotary sample valve.  Rotation of the valve by 45 deg then introduces the reproducible volume into the mobile phase.  Errors due to sample size can be reduced to 0.

Column Configurations  Two general types of columns are encountered in gas chromatography. or Teflon. . glass. In order to fit into an oven for thermostating.  Chromatographic columns vary in length from less than 2 m to 50 m or more. packed and open tubular. fused silica. or capillary. they are usually formed as coils having diameters of 10 to 30 cm. They are constructed of stainless steel.

The optimum column temperature depends upon the boiling point of the sample and the degree of separation required.  Thus.Column Ovens  Column temperature is an important variable that must be controlled to a few tenths of a degree for precise work. the column is ordinarily housed in a thermostated oven. .

 For samples with a broad boiling range. whereby the column temperature is increased either continuously or in steps as the separation proceeds. a temperature equal to or slightly above the average boiling point of a sample results in a reasonable elution time (2 to 30 min). it is often desirable to employ temperature programming. .Column Ovens  Roughly.

A temperature range from room temperature to at least 400oC.Detection Systems Properties of the Ideal Detector: The ideal detector for gas chromatography has the following properties: 1. 3. Adequate sensitivity 2. Good stability and reproducibility. . 4. A linear response to solutes that extends over several orders of magnitude.

8. Similarity in response toward all solutes or a highly selective response toward one or more classes of solutes.Characteristics of the Ideal Detector 5. . High reliability and ease of use. 6. A short response time that is independent of flow rate. Nondestructive of sample. 7.

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produce ions and electrons that can conduct electricity through the flame.Flame Ionization Detectors (FID) The flame ionization detector is the most widely used and generally applicable detector for gas chromatography. when pyrolyzed at the temperature of a hydrogen/air flame.  The effluent from the column is mixed with hydrogen and air and then ignited electrically. .  Most organic compounds.

 A disadvantage of the flame ionization detector is that . large linear response range (~107). and low noise. it is destructive of sample.  The resulting current (~10-12 A) is then measured.  The flame ionization detector exhibits a high sensitivity (~10-13 g/s).Flame Ionization Detectors (FID)  A potential of a few hundred volts is applied.

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.GAS CHROMATOGRAPHIC COLUMNS Open tubular Columns Open tubular. or capillary. namely wall—coated open tubular (WCOT) and support-coated open tubular (SCOT). columns are of two basic types.

aluminum). metal (stainless steel. . copper. or Teflon tubes that typically have lengths of 2 to 3 m and inside diameters of 2 to 4 mm.Packed Columns Packed columns are fabricated from glass.

which is made up of the skeletons of thousands of species of single-celled plants (diatoms) that inhabited ancient lakes and seas.Solid Support Materials The most widely used support material is prepared from naturally occurring diatomaceous earth. .

The pressure difference required to maintain a given flow rate of carrier gas. varies inversely as the square of the particle diameter.Particle Size of Supports The efficiency of a gas-chromatographic column increases rapidly with decreasing particle diameter of the packing. however. .

(4)solvent characteristics such that k` and  values for the solutes to be resolved fall within a suitable range.The Stationary Phase Desirable properties for the immobilized liquid phase in a gas-liquid chromatographic column include: (1)low volatility (ideally. the boiling point of the liquid should be at 100oC higher than the maximum operating temperature for the column). (3)chemical inertness. . (2)thermal stability.

Reliability is directly related to the control of variables. An accuracy of 1% relative is attainable under carefully controlled conditions.Quantitative Analysis The detector signal from a gas-liquid chromatographic column has had wide use for quantitative and semiquantitative analyses. . the nature of the sample also plays a part in determining the potential accuracy.

Interfacing Gas Chromatography with Spectroscopic Methods Gas chromatography is often coupled with the selective techniques of spectroscopy. thus giving socalled hyphenated methods that provide the chemist with powerful tools for identifying the components of complex mixtures. .

For packed columns and megabore capillary columns however.Chromatography/Mass Spectrometry (GC/MS) The flow rate from capillary columns is generally low enough that the column output can be fed directly into the ionization chamber of the mass spectrometer. a jet separator must be employed to remove most of the carrier gas from the analyte. .

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