GAS CHROMATOGRAPHY

GROUP 2 (2A BC)

AQUINO, MA. GRACIELA I.

BADUA, ALYSSA A.

BELARDO, ALYSSA JERSEY S.

CABASAG, ALTHEA SUZERANE D.

CANTAL, IRINE NICOLE A.

INTRODUCTION
 GAS CHROMATOGRAPHY

A technique for separating chemical substances

that relies on differences in partitioning behavior between
a flowing mobile phase and a stationary phase to
separate the components in a mixture.
 GAS CHROMATOGRAPHY
Mobile phase: inert gas

Stationary phase: thin layer of inert liquid or solid

Used to analyze volatile substances in a sample.

Measures the content of various components in a

sample

Simple, sensitive, and effective

 GAS CHROMATOGRAPHY
Consists of:
Injection port
Column
Carrier gas flow control equipment
Ovens and heaters
Detector
Used for quantitative and qualitative of mixtures
Used for purification of compounds
For the determination of such thermochemical constants
as heats of solutions and vaporization
 GAS CHROMATOGRAPHY
Types of Gas Chromatography

1. Gas-Solid Chromatography (GSC)

Solid stationary phase on which retention of analytes
is the consequence of physical adsorption.

2. Gas-Liquid Chromatography (GLC)

Separation of ions or molecules that are dissolved in
a solvent.
HISTORY
 1941 - Martin and Synge ; gas-liquid chromatography
1955 - First commercial gas-liquid chromatograph
1970s - Electronic integrators and computer-based data-
processing equipment became common.
1980s - Automatic control of instrument parameters
- High-performance instruments ; moderate costs
- Open tubular columns
2002 - Clarus 500 gas chromatograph and GC/MS lines ;
perkin-elmer
- First touch-screen display based graphical user interface.
 ADVANCEMENTS IN GC

High-speed Gas Chromatography

Miniaturized GC Systems

Multidimensional Gas Chromatography

INSTRUMENTATION
Figure 1. Schematic Diagram of Gas Chromatography
 I. CARRIER GAS
Inert
Free from impurities
No impact on partitioning between mobile and stationary
phase
Examples of carrier gas:
1. Helium - commonly used, expensive
2. Nitrogen - high efficiency, long run time
3. Hydrogen - shortest analysis time
 II. FLOW REGULATORS
Control the flow rate of gas

Retention time - dictates which molecule comes first or

last which helps the detector identify the number of
substances present
 III. INJECTION CHAMBER

Figure 2. Cross-sectional view of a microflash vaporizer direct injector.

 IV. COLUMN
Column where separation of the components of the
analyte happens.
PACKED COLUMN
Fabricated from glass or metal tubing
2 to 3 m long; diameters of 2 to 4 mm (larger diameter
than capillary column)
Densely packed with a uniform, finely divided packing
material or solid support (such as diatomaceous earth)
that is coated with a thin layer of liquid stationary phase
 IV. COLUMN
CAPILLARY COLUMN (OPEN TUBULAR COLUMN)
Types of Capillary Column
1. Wall-coated open tubular (WCOT) columns, the
interior of the capillary tube is coated with a thin layer of
liquid
2. Support-coated open tubular (SCOT) columns, the
interior is lined with a thin film of a solid support material,
such as diatomaceous earth, on which the liquid
stationary phase is adsorbed.
 IV. COLUMN
3. Fused-silica open tubular (FSOT) column is the
most widely used in GC. It is made with specially
purified silica that contains minimal amounts of metal
oxides. They have thinner walls and more flexible than
glass columns.
 IV. COLUMN
How separation happens

Each component may:

1. Condense on the stationary phase
2. Dissolve in the liquid on the surface of stationary
phase
3. Remain in the gas phase
 IV. COLUMN

A B C D E
WCOT SCOT PLOT FSOT PACKED COLUMN

Figure 3. Different types of column

 V. LIQUID STATIONARY PHASE
The polarity of the stationary phase should match that of the
analyte
Thick films are used for high volatile analytes for longer retention
and better separation
Thin films are used for less volatile analytes
Properties of liquid stationary phase:
1. Low volatility: the bp of the liquid should be at least 100C
higher than the operating conditions for the column
2. Thermal stability
3. Chemical inertness
4. K and of solvent should fall within a suitable range
 VI. DETECTORS
Detector device located at the end of the column which
measures the components of the mixture as the elution
happens.
Characteristics of the Ideal Detector
1. Adequate sensitivity of 108 to 1015 g solute/s
2. Good stability and reproducibility
3. Linear response to solutes that extends to several orders of
magnitude
4. Temperature range of room temp to at least 400C
5. Short response time that is independent of the flow rate
6. High reliability and ease of use
7. Similarity in response to all solutes
8. Nondestructive of the sample
 VI. DETECTORS
Flame Ionization Detector (FID)
most common and generally applicable
measures hydrocarbon concentration
effluent is directed into a small air/hydrogen flame
has high sensitivity (~1015 g/s) and large linear response
insensitive to noncombustible gases like H2O, CO2, SO2 and nox
carbonyl, alcohol, halogen and amines yield fewer or no ions at all in
flame
Advantage: changes in flow rate of the mobile phase have little effect
in detector response
Disadvantage: destructive; it also requires additional gases and
controllers
 VI. DETECTORS
FID

Sample injection system

Data system GC

Figure 4. GC/FID System

 VI. DETECTORS
Other GC Detectors:
1. Thermal Conductivity Detector(TCD) universal
detector
2. Electron capture (EC) halogenated compounds
3. Mass spectrometer (MS) tunable for any species
APPLICATIONS
 APPLICATIONS
1. Quantifications of drugs and their
metabolites.
Used for both pharmaceutical and forensic
applications
 APPLICATIONS
2. Blood alcohol analysis
Determines the blood alcohol content
Commonly performed in forensic laboratories
Packed columns applications are most commonly
used in this analysis
Figure 5. Chromatogram of analysis of blood alcohols in
human plasma
REFERENCES
Skoog, D. A., West, D. M., Holler, F. J., & Crouch, S. R.
(2016). Fundamentals of Analytical Chemistry (9th Ed.). Bonifacio Global
City: Cengage Learning.
https://www.sigmaaldrich.com/content/dam/sigma-
aldrich/docs/promo_not_indexed/general_information/1/gc-09-carrier-
gases-gc.pdf
https://www.britannica.com/biography/a-j-p-martin#ref13467
http://www.sciencedirect.com/science/article/pii/s0165993602008063
http://www.shimadzu.com/an/gc/index.html
http://chem.libretexts.org/core/analytical_chemistry/instrumental_analysi
s/chromatography/gas_chromatography
 http://hiq.linde-
gas.com/en/analytical_methods/gas_chromatography/index.html
http://www.sigmaaldrich.com/content/dam/sigma-
aldrich/docs/supelco/general_information/1/t411126h.pdf
http://www.labmanager.com/lab-product/2010/02/evolution-of-gas-
chromatography#.wi9fftj961s
http://www.chemguide.co.uk/analysis/chromatography/gas.html
http://www.bbc.co.uk/schools/gcsebitesize/science/triple_ocr_21c/furt
her_chemistry/chromatography/revision/5/