After students spend a lab session learning the basic principles of a gas chromatography and the importance of temperature programming, they are given a sample with seven compounds and an example chromatogram of an isothermal GC-analysis. Students are required, with a limited amount of time and trials, to improve the method from an isothermal analysis to a programmed temperature analysis with good resolution, but in the shortest possible time. The instructions given to them are shown below:
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Introduction:
An example chromatogram (see Fig. 1) shows the results of an isothermal (80°C) analysis of the mixture of 7 compounds. Although all compounds are well separated, the analysis time is quite long.
Experiment 1C: Optimisation of GC separation
(internal competition)
Introduction:
An example chromatogram (see Fig. 1) shows the results of an isothermal (80°C) analysis of the mixture of 7 compounds. Although all compounds are well separated, the analysis time is quite long.
It is your task to develop a method through temperature programming to separate out all 7 compounds in the shortest possible analysis time. How you develop your method is all up to you as a group. The group who managed to get the best separation and the shortest analysis time will receive a prize!
In this laboratory session you will be able to
- apply the knowledge of the lectures and lab session 1 to solve a problem
- develop your own method in which your aim is to separate out all 7 compounds within a mixture in the shortest possible analysis time
- achieve a resolution of minimal 1.5 (baseline separation) between peaks 2/3 and 4/5
Develop a programmed oven temperature program that is most suitable for the analysis of mixture B containing the 7 compounds.
1) What GC parameters can/should be varied
- Initial oven temperature
- Hold
- Temperature ramp(s)
- Final oven temperature
- You are only allowed to inject your sample a maximum of 3 times!
- Maximum final oven temperature is 270°C
- A good separation means that all resolutions should be at least 1.50
- Analysis time = retention time of the last compound
- Only inject when the GC is in ‘ready’ status
- Start the GC temperature programming at the same time as the data collection on LoggerPro
- You will need to present your method in a short presentation.
~~ Good Luck!! ~~
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I do this in the beginning of the module (week 2 or 3) and it does help to get students to discuss problems with each other or with me throughout the module.
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Learning by Competition by Falko Drijfhout, Keele University is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.