EXPERIMENT 3: ANALYSIS OF CHEMICAL MISTURES USING GAS

CHROMATOGRAPHY (GC)

Part B: Qualitative Separation And Determination Of Alcohols Using Isotherm And

Programmed Temperature Methods

Objectives:

Upon completion of this experiment, students should be able to:

1. To separate mixture of alcohols (methanol, ethanol and propanol) using isotherm

method
2. To separate mixture of alcohols (methanol, ethanol and propanol) using programmed
temperature method
3. To identify of alcohol peaks (retention time, tR) using isotherm method
4. To compare chromatogram obtained by using isotherm and programmed temperature
methods

Introduction:

The column temperature is a compromise between speed, sensitivity and resolution. At

high column temperature, the sample components spend most of their time in the gas
phase and so they are eluted quickly, but resolution is poor. At low temperature, they
spend more time in the stationary phase and elute slowly, resolution is increased but
sensitivity is decreased due to increasing spreading of the peaks. Some separations can be
facilitated by temperature programming. The temperature is automatically increased at
preselected rate during the running of the chromatogram. Another method is to run
chromatogram at a chosen temperature. This method is known as isotherm temperature.

Chemicals and Apparatus:

Chemicals:

Standard solution of methanol, ethanol and propanol

Mixture of alcohols (methanol, ethanol and propanol)

Apparatus:

Micro syringe

Procedure:

Isotherm method

1. The temperature of oven was set to 150℃. The temperature was allowed to stable
2. 1.0 μL amount of each methanol, ethanol and propanol was injected.
Chromatograms of each separate components was obtained
3. 1.0 μL amount of standard mixture of methanol, ethanol and propanol was
injected. Every single peak of the chromatogram was identified. Comments on the
separation (resolution of the chromatogram peaks) was given

Programmed Temperature Method

1. The initial temperature of oven as 60℃ and its final temperature as 100℃ was
set. The temperature was allowed to stable
2. 1.0 μL amount of the standard mixture of methanol, ethanol and propanol was
injected. Every single peak of the chromatogram was identified. Comments on
the separation (resolution of the chromatogram peaks) obtained was given and
compared to the chromatogram obtained using isotherm method

Results:

Retention time of standard alcohol solutions using isotherm method

Component Dead time, tM (min) Retention time, tR (min)

Methanol
Ethanol
Propanol
Retention time of standard alcohol solutions using programmed temperature method

Component Dead time, tM (min) Retention time, tR (min)

Methanol
Ethanol
Propanol

Retention time of alcohols in mixture separated by using isotherm and programmed

temperature methods

Isotherm Programmed
Component tR (min) Component tR (min)
Methanol Methanol
Ethanol Ethanol
Propanol Propanol