Romatographic Methods of Analysis: Section: 5 Gas Chromatography (GC)

Chromatographic Methods
of Analysis
Section: 5 Gas Chromatography
(GC)
Prof. Tarek A. Fayed

Gas Chromatography (GC)
 In gas chromatography, the sample is vaporized and
injected onto the head of a chromatographic column.
Elution is made by the flow of an inert gas as a mobile
phase (He, N2 and sometimes H2).
 The mobile phase, does not interact with molecules of
the analyte (components to be separated); its function is
only to transport the analyte through the column, so it is
called a carrier gas.
There are two type of such technique:
1- Gas-liquid chromatography (GLC) which is based upon
the partition of the components between the gaseous
mobile phase and a nonvolatile liquid phase immobilized
on the surface of an inert solid support .
Most common stationary phase in GLC:
1- For separation of mixture of polar compounds poly-
3
ethylene glycol is used.
2. For separation of mixtures of non-polar compounds
polymer of methylsilicone is used.
2- Gas solid chromatography (GSC) which is based on the

adsorption of components on the solid stationary phase
(as silica or alumina).
 The principle of GC is the separation of volatile

components based on the difference in adsorption
characters of components or partition of them between the
carrier gas and the solid or liquid stationary phase,
respectively.
Instrument for GC (gas chromatograph)
Components of a Gas Chromatograph
Gas Supply: Cylinder containing a chemically inert gas like
N2, He or CO2 , the flow rate is controlled by a regulator.
Sample Injector: Contains heated chamber through which
the sample is injected by a micro-syringe (from steel or
Teflon). Sample sizes vary from about 1/10 µl to 20 µl
Column: Typically stainless or glass, 1.5 - 10 m long and 2 -
4 mm in diameter. packed with small uniform size, inert
support coated with thin film of nonvolatile liquid. Column is
housed in a thermo-stated oven. Temperature must be
strictly controlled, slightly higher than its boiling point of
components.
Detector: There are several types of detectors to monitor the
outlet of the column, each respond to different compounds
or properties.
Recorder: Converts the detector signal into a sequence of
peaks (known as a chromatogram).
 Detectors:
They are used to indicate the presence and measure the
amount of the components in the column effluent.
Examples of the commonly used detectors are:
1- Thermal Conductivity Detector (TCD):
 Measures the changes of thermal conductivity of the
carrier gas.
 Non specific (responds to
all compounds) with
suitable sensitivity.
 Good linear range of signal
and stable signal.
 Nondestructive detector
 High detection limit.
2- Flame Ionization Detector (FID)
Coaxial cable to
Teflon insulating ring Analog to Digital
converter
Gas outlet
Collector
Ions
Flame
Sintered disk
Platinum jet
H2-air
Gas inlet Column effluent

 In FID, high temperature of hydrogen flame (H2
+ O2 + N2) ionizes compounds eluted from
column into flame.
The ions collected on collector or electrode and
were recorded on recorder due to electric
current.
 Responds to compounds that produce ions
when burned in an H2-air flame (all
hydrocarbons).
 Small or no response to inert gasses.
 High sensitivity, linear from the minimum
detectable limit through concentrations to 10-7.
 Destructive for detected components.
3- Electron capture detector ECD
 In ECD, electrons from
radioactive source is captured by
organic molecules and decrease
current.
 Simple and reliable detector.
 Sensitive to electronegative
groups (halogens, peroxides and
cyano or nitro-derivatives)
as in pesticide, Insecticides, vinyl
chloride, and fluorocarbons in
foods.
Insensitive to amines or alcohols
 Non-destructive and low
detection limit (10-12).
Factors affecting separation by GC
1- Nature of stationary phase:
 Solid with adsorption characters or non-volatile liquid.
 Particles size which controls the surface area (300-600 or 150-300 m). The
efficiency of a gas-chromatographic column increases rapidly with
decreasing particle size.
2- Carrier gas:
 Flow rate; high flow rate leads to higher speed and low resolution due to
longitudinal diffusion.
 Pressure; the pressure difference between column in and out, required to
maintain a given flow rate of carrier gas is 1 atm.
3- Nature of sample:
 More volatile compounds are easily to be carried by carrier gas.
 Injection time (longer time leads to low resolution).
 Polarity of compounds and column (like dissolves like).
4- temperature:
 As column temperature increases, faster movement and lesser
separation takes place.
 Temperature of the column should be controlled near the boiling
point of the components.
5- Column dimensions:
 Length of the column- greater separation using longer column.
 Diameter of column; small diameter leads to slow low rate and high
resolution.
Applications of GC
1- Qualitative Analysis
 Gas chromatograms are widely used as criteria of purity
for organic compounds. impurities, if present, are
revealed by the appearance of additional peaks. The
components elapsed from the GC are subjected to
analysis by IR or mass spectrometer to determine their
structure, molecular weight and fragmentation pattern
for the identification purpose.
 It can also be made by determination of retention time.
The identification based on the comparison of the

retention time of the substance not only with one
standard but with series of hydrocarbons (n-paraffins
CnH2n+2).
GC Chromatogram of hydrocarbon mixture
 Compound Boiling Point (0C) Boiling Point (0C)

 pentane 36 toluene 110
 hexane 69 4-methyl-2-pentanone 117
 cyclohexane 80 octane 126
 isooctane 99
Identification of unknown compounds by comparison of retention time
Dr Gihan Gawish
2- Quantitative Analysis
A)From the area under peak: The area under peak is proportional
to the amount (moles) of the compounds eluted.
 The molar percentage composition of a mixture can be approximated
by comparing the relative areas of the peaks in the chromatogram.
Determination of the area under peak
 Multiply the height of peak (in mm) above the baseline
by the width of the peak at half the height.
 Baseline is a straight line
connecting side arms of
Baseline
the peak.
 Add the individual areas
to get the total area
 Divide each area by total
area to get mole fraction
 Multiply mole fraction by
Baseline
100 to get adjusted mole %

B) Internal Standard Method
 In this approach, an internal standard is added to the
sample, and the response from the analyte peak is
compared to the internal standard.
 Response Factor (RF)
The response factor accounts for differences in the
detector response between the analyte and standard. It
is measured by injecting a mixture containing known
amounts of analyte and standard. For some analyte X,
the response factor is
Ax, Ais are the peak areas for  Ax   Ax 
   
the analyte and internal standard. 
Rx / is 
m x  Aix 

mx, mis are the masses of  Ais   mx 
   
 m is   m is 
analyte and internal standard.
17
C) Calibration Curve with Internal Standard
Standards
• Each contains fixed mass of
internal standard, various
masses of std analyte
• Calibration curve shows
linear response.
Unknown
• Add known amount of internal
standard
• Inject and measure Ax/Ais
• Determine cx/cis for your
unknown from calibration Ax Ais  ( y intercept)
A A Rx / is 
curve. Since cis is known, cx Rx / is  x is c x cis
for your unknown is simply c x cis
cx = (cx/cis)cis
Examples for GC applications:
1- Forensic Applications
 Analysis of bodily fluids (for example: semen or urine)
to test for illegal substances such as alcohols.
 Test fibers and blood recovered at a crime scene.
 Detect residue from explosives and ignitable fluids/
presence of accelerants
2- Separation of racemic mixtures in drugs industry
using optically active stationary phase
3- Separation and determination of hydrocarbons in oil
industry.
4- Separation and determination of pesticides in foods,
water and soil.
5- Extraction and analysis of carbonyl compounds (like
aldehydes) from natural products (as sunflower oils),
which are formed due to lipid peroxidation.
6- Quality and production control of diesel fuel, beer
constituents and aditives in foods and soft-drinks.

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Chromatographic Methods

Prof. Tarek A. Fayed

2- Gas solid chromatography (GSC) which is based on the

 The principle of GC is the separation of volatile

Gas inlet Column effluent

The identification based on the comparison of the

 Compound Boiling Point (0C) Boiling Point (0C)

100 to get adjusted mole %

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