GAS LIQUID CHROMATOGRAPHY

Gas Liquid Chromatography

• Principles
Partition of molecules between gas (mobile
phase) and liquid (stationary phase).
 Most Common Stationary Phases

1. Separation of mixture of polar compounds

Carbowax 20M (polyethylene glycol)

2. Separation of mixtures of non-polar compounds

OV101 or SE-30 (polymer of methylsilicone)

3. Methylester of fatty acids

DEGS (diethylene glycol succinate)
 Gas Chromatography

Filters/Traps Data system

H

RESET

Regulators Syringe/Sampler

Inlets

Detectors
• gas system
Gas Carrier
Hydrogen

• inlet
Air

Column
• column
• detector
• data system
Schematic Diagram of Gas Chromatography
Gas Chromatography Application
 Semi-Quantitative Analysis of Fatty Acids

C18
10

C16 8

Peak Area
Response

6
Detector

C14 4

0.5 1.0 1.5 2.0 2.5 3.0

Sample Concentration (mg/ml)
Retention Time

C1
4
The content %of C14fatty acids = ∗1
0
C + C+
1
61
C 8
1
4

= the content % of C fatty

14 acids
Advantages of Gas Chromatography

• Very good separation

• Time (analysis is short)
• Small sample is needed - µ l
• Good detection system
• Quantitatively analyzed
Disadvantages of Gas Chromatography
Material has to be volatilized at 250C without decomposition.

Fatty Acids Methylester

O O
R C OH + CH3OH + H2SO4 R C O CH3
Reflux Volatile in Gas
Chromatography
O
CH2 O C R

O CH3ONa O
CH O C R + CH3OH 3 R C O CH3
Volatile in Gas
O Chromatography
CH2 O C R
Gas Chromatogram of Methyl Esters of Fatty Acids
Effects of OH groups of Carbohydrates

6
CH OH
2
O
5
4 1
OH
HO
OH
3 2
OH
Derivation of Glucose with Trimethylchlorosilane
6
CH2OH
O CH 3
5
4
OH 1 + 5Cl Si CH 3
HO
3 2 OH CH 3
OH
Glucose Trimethylchlorosilane
6
CH2O-Si(CH3)3
O
5
4 + 5HCl
O-Si(CH ) 1
3 3
(CH3)3-Si-O
3 2 O-Si(CH3)3
O-Si(CH3)3
Effects of Derivation

• Time consumption
• Side reaction
• Loss of sample