Method Development 3
Advanced Operation 43
Developing and Improving the Method
This section discusses how to improve a method by using
various 7697A HS features. It provides useful tips and
background information that will help you develop methods
using the HS. It is not a general discussion of headspace
chromatography, but rather a collection of information to
help you use the Agilent 7697A to best advantage.
Using parameter increment
The goal of the initial method is to safely get results—any
results. Once you have determined that a method safely
extracts sufficient sample that can be analyzed by the GC
(or GC/MS), then next step is typically to empirically
determine the equilibration temperature, time, and shaking
level that provide the best optimization for your needs.
To do this, use the parameter increment feature of the HS.
Parameter increment will increase oven temperature, vial
equilibration time, or vial shaking level by a set amount in
consecutive runs.
To use parameter increment:
1 Load the desired method.
2 Press [Adv Function], scroll to Method development, then
press [Enter].
3 With Parameter increment selected, press [Mode/Type].
4 Select Tem peratu re, Vial shaking, or Vial equilibration hold time.
5 Enter the appropriate parameters. See “Oven
temperature”, “Vial equilibration time”, or “Vial shaking
level” below for details.
6 Save (store) the method.
7 Determine the number of sample vials needed.
• The parameter will increment until it exceeds the
specified upper limit. (For an example, see Table 10.)
• Divide the range by the increment and round up.
8 Prepare the sample vials and load them into the tray (or
carousel).
9 Create a sequence to run each vial using the parameter
increment method.
10 Press [Start].
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