This course has been designed for those who are experience in GC and who are now looking to develop their experience and understanding of method development. During the course we will assume that you are familiar with the basic theories of gas phase chromatographic separations, but we’ll also revisit some theory to underpin the teaching.
This course is approved by the Royal Society of Chemistry & American Chemical Society - Division of Analytical Chemistry.
We begin by discussing how to set analytical objectives, because, in the words of the Wizard of Oz, if you don’t know where you are going, how do you know when you’ve arrived! This will involve assessment of the sample matrix and analyte chemistry (where known) and their influence on designing methods and setting analytical objectives.
We’ll look at the sample preparation options available to us and the types of preparation that might be required for various inlet types and detection techniques. We also begin our discussion on selecting the correct mode of chromatography for our separation and examine some of the stationary phase chemistries available to today’s method developers.
In our second session we begin to explore the choices available for sampling and sample introduction. We discuss in-depth the choices for split and splitless injection and the important variables associated with each of these techniques.
We will consider important choices such as inlet liner design and selection, factors which determine split ratio, and unique splitless injection parameters such as initial oven temperature and purge time.
We will also consider how to avoid insidious issues such as discrimination and backflash. In this session we will also investigate headspace analysis and other sampling techniques.
In this session we investigate the important choices which govern the selection of GC column dimensions and how to optimize efficiency and analysis time.
We also discuss sample screening methods to investigate the retention behavior of the analytes and make some initial decisions regarding the requirements for the temperature program.
Using temperature programming theory, we investigate how to optimize the temperature program parameters, such as initial and final temperature and the slope of the temperature gradient. We discuss the use of mid ramp holds for separating critical peak pairs within the analysis. We also begin our discussion on GC detectors by examining the range of detector types available and the factors which govern detector selection.
In the final session we take an in-depth look at various popular detectors for GC and highlight the important variables which govern response and dictate sensitivity.
We look at the full range of ionizing detectors, including mass spectrometric detectors as well as electron capture and thermal conductivity detectors and highlight the key method development decisions associated with each detector.
We conclude the course with an example method development which will serve to reinforce your learning and highlight the key method development decisions and optimization processes associated with logical method development for capillary GC.