GAS

CHROMATOGRAPHY
Skoog

For separation of volatile substances

Sample is injected into the gas chromatograph.
Mobile phase (carrier gas) moves through column
Stationary phase that contains a wall coated or
granular solid coated.
Differential migration of solutes, thus leading to
separation
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Martin and James in 1941

Commercialization 1955
Routine lab tool
Good only for volatile compounds or those, which
can be made volatile by suitable derivatization
methods or pyrolysis.

For both qualitative and quantitative analysis.

Qualitative analysis : Comparison of retention times
- to identify materials in the sample
Quantitative analysis : by measurement of either
peak height or peak area

GC
GSC
GLC

Gas - Solid Chromatography (GSC)

o Stationary phase- silica or alumina
o Mobile phase

- carrier gas

o MECHANISM :

o Physical adsorption.
o APPLICATION :

o For separation and analysis of gases.

o For

trace analysis of organic and inorganic compounds

o LIMITATIONS :

o Marginal use because of tailing (??)

o Low MW mass separation
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Gas - Liquid Chromatography (GLC)

o Stationary phase - liquid with very low volatility
o Mobile phase - gas
o Most widely used technique for separation of volatile species
o Wide variety of stationary phases with contrasting selectivity
o Easy column preparation

PRINCIPLE OF GLC
RETENTION VOLUME
VR =tR F
F-flow rate

Instrumentation
o 1980 Column temperature, flow rates, and sample injection
o High performance
o Moderate costs
o Separation in short times
o Cost $1000 to $ 50,000

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SAMPLE
GAS, SOLID OR LIQUID

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The Carrier Gas

o Mobile phase - chemically inert [He, Ar, H2]
o Gas in pressurized tanks
o Pressure regulators, gauges, flow meters- control flow rate of gas
o Carrier gas system contains molecular sieve to remove
impurities and water

A carrier gas should have the following properties:

1. Highly pure
2. Inert at high temperatures
3. Compatible with the detector
4. A cheap and available carrier gas is an advantage

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To Waste or Flow
Meter
Two-Stage
Regulator

Syringe

Detector

Injector

Flow Controller

Carrier Gas
Cylinder

Column

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FLOW RATE
Two-stage pressure regulator at gas cylinder
Inlet pressure- 10 to 50 psi [F = 25-150 mL/min]
To detect flow rate :
1. Soap bubble flow meter
Soap film passed through two graduations
in a burette
2.Electronic flow meter

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Injectors
Sample must be of suitable size and introduced as
plug of vapor
Slow injection or oversize samples cause band
spreading and poor resolution

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Calibrated micro syringes / Septum type injectors

CONSTRUCTION : Glass tube
USE: To inject liquid samples through a rubber or silicone diaphragm or septum
into heated sample port at head of column
Sample port is at 50C above boiling point of least volatile component of
sample

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SAMPLE SIZE
Sample size - tenths of microlitre to 20L
SAMPLE SPLITTER : delivers small known fraction of sample and
remaining excess fraction as waste
On-column inlet entire sample loaded- vaporised by temperature
programming of column or inlet
Autoinjectors- automatic sampling trays
Improves precision

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SAMPLE INJECTION

TO FILL SAMPLE

SAMPLE INTRODUCTION TO COLUMN

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Column Configurations and

Ovens
Packed or
Open tubular
Packed columns : most common
short (1-5 meters)
Open tubular : called as capillary
length is 30-100 meters
fast developments
good efficiency
speed

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Stainless steel or glass filled with fused silica

Coils have diameters of 10-30 cm
COLUMN TEMPERATURE :
Thermostatted oven adjusted so that it is close to the average boiling
point of the sample mixture.
Temperature programming for better separations.
The oven temperature should be stable and easily changed in order to
obtain reproducible results
Elution time > 2 to 30 min
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TEMPERATURE
PROGRAMMING

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GC COLUMNS
COLUMN SIZE
PACKED :Inner dia.: 2-4 mm
Glass or metal tubing
2-3 m long
Coils of 15 cm
Convenient thermostatting
SP- 0.05 to 1 m
OPEN TUBULAR :
Inner dia.: 0.32 mm and 0.25 mm

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OPEN TUBULAR COLUMN or capillary

WALL-COATED OPEN TUBULAR
Capillary tubes coated with thin
layer of SP
SUPPORT-COATED OPEN
TUBULAR
Capillary tubes coated with thin
film(~30 m) of SP

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GC STATIONARY PHASES
Diatomaceous earth
Silica
No perfect material found
Support particle size 60-80 mesh( 250-170 m) or 80-100 mesh (170-149 m)

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