Frontier EGA/PY-3030D - Page 79

Ver.1.36
8-2
Fig. 8.1 Test conditions and a typical EGA thermogram
Analytical conditions
ITF tube : EGA tube
(deactivated metal capillary, L=2.5 m, id.=0.15 mm,
no stationary phase)
Column flow : 1.0 ml/min
Split ratio : 1/100
Oven temp. : 300°C (isothermal)
Injector temp. : 300°C
Py furnace temp. : 100 - 550°C (20°C/min)
Py-GC ITF temp. : 300°C (AUTO mode)
Sample : Polystyrene (contains 5 wt% methyl stearate)
Sample wt. : 125 µg (5µl of 25 µg/µl dichloromethane solution)
Sample cup : Eco-Cup LF
Detector : MS or FID
GC/MS ITF temp. : 300°C
Scan range : 29 - 350 (m/z)
Scan speed : 0.1 scan/sec
Peak apex temperature
(RSD ≤ 0.3%, n=3)
Methyl Stearate
500
400
200
100
Polystyrene
300
Fig. 8.2 Test conditions and a typical check-out sample pyrogram
Analytical conditions
Separation column : Ultra ALLOY
+
-5
(5% phenyl 95% dimehtylpolysiloxane
L=30m, id.=0.25mm, df=0.25 µm)
Column flow : 1.0ml/min
Split ratio : 1/100
Oven temp. : 70 - 320°C (20°C/min, 1 min hold)
Injector temp. : 300°C
Py furnace temp. : 550°C
Py-GC ITF temp. : 300°C
Sample : Polystyrene (contains 5 wt% methyl stearate)
Sample wt. : 25 µg (5µl of 5µg/µl dichloromethane solution)
Sample cup : Eco-Cup LF (single cup used)
Detector : MS (200V lower than that of Autotune)
GC/MS ITF temp.: 300°C
Scan range : 29 – 350 (m/z)
Scan speed : 3 scans/sec or greater
100
200
300 m/z
91
117
207
194
312
100
200
300 m/z
74
87
143
298
255
199
100
200 m/z
91
208
104
130
Mass spectra of maijor peaks
SS
Me-Stearate
SSS
Peak ratio of SSS / Me-Stearate
RSD ≤ 2% (n=3)
Me-Stearate
SSS
Styrene monomer
SS
10 min
5