Ver.1.36
CHAPTER 5 FOUR ANALYSIS METHODS AND SAMPLE
PREPARATION
Four analysis methods (Single-Shot, Double-Shot, evolved gas analysis, and Heart-Cut EGA analysis)
are described. Refer to Chapter 4 for details about settings and operations. Sampling techniques are
also described here.
5.1 SINGLE-SHOT ANALYSIS
This method is also called flash pyrolysis. The sample is placed in a sample cup which is then
attached to the sampler. The sampler is attached to the Multi-Shot pyrolyzer. Pyrolysis occurs when
the cup is released and “free falls” into the pyrolyzer furnace which is at the pre-selected pyrolysis
temperature. The gases generated in the furnace are swept into the splitter by the carrier gas. The
sample vapors are split; a portion going to the analytical column and a portion exiting via the split vent.
A typical instrument configuration for a Py-GC/MS system is shown in Fig. 5.1.
An example of a Single-Shot analysis using the polystyrene solution is described below. The test
sample vial contains 2.5 mg of polystyrene and approx. 5% (wt/wt) of methyl stearate. Adding 0.5 mL
of dichloromethane, benzene, or toluene makes a test solution (5 µg/µL). The sample used here is a
dichloromethane solution of polystyrene (5 µg/µl) with methyl stearate.
STEP1 Install the 30 m capillary column provided with the 3030D pyrolyzer.
STEP2 Set the pyrolysis and GC conditions (see Fig. 5.3)
(1) Set the interface temperature (ITF TEMP) to “Auto” mode.
(2) Set the pyrolysis temperature in “Single-Shot Analysis” screen.
Fig. 5.1 Typical instrument configuration for Py-GC/MS
Multi-Shot Pyrolyzer (550°C)
Split/splitless injection port
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