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OVIs by Dynamic Headspace and Gerstel MACH on Rtx-624 (G43) and Rtx-WAX (G16)

ColumnsRtx-624 20 m, 0.18 mm ID, 1.00 µm (cat.# 40924)
and Rtx-WAX (G16) 20 m, 0.18 mm ID, 0.4 µm (custom)
using IP deactivated guard column 5 m, 0.32 mm ID (cat.# 10044)
with Universal “Y” Press-Tight connector (cat.# 20405)
SampleResidual solvents Class 2 - mix A (cat.# 36271)
Residual solvents Class 2 - mix B (cat.# 36272)
Diluent:0.5 mL DI water/~0.2 g sodium sulfate in 20 mL headspace vial; components at 0.10 - 6.00 µg
Injectionheadspace-trap split (split ratio 20:1)
Headspace-Trap
Instrument:Tekmar HT3
Inj. Temp.:220 °C
Transfer Line Temp.:220 °C
Valve Oven Temp.:220 °C
Standby flow rate:50 mL/min
Trap Standby Temp:40 °C
Trap Sweep Temp:40 °C
Preheat Mixer:On
Preheat Mixer Time:2.0 min
Preheat Mixing Level:5
Preheat Mixer Stabilize Time:0.5 min
Sample Temp.:80 °C
Sweep Flow Rate:75 mL/min
Sweep Flow Time:5.0 min
Dry Purge: 10.0 min, flow 100 mL/min @ 25 °C
Desorb Preheat Temp:245 °C
Desorb: 1.0 min @ 250 °C
Trap Bake Temp:260 °C
Trap Bake Time:6.0 min
Trap Bake Flow:450 mL/min
Oven
Oven Temp.:250 °C
Carrier GasHe
DetectorFID @ 250 °C
Make-up Gas Flow Rate:45 mL/min
InstrumentAgilent 6890 with Gerstel Modular Accelerated Column Heater (MACH)
NotesSample preheat time: 15.00 min

Flow rate: constant flow; column 1: 0.85 mL/min; column 2: 0.99 mL/min

Gerstel temps.:

Column 1: 50 °C (2 min) to 80 °C at 20 °C/min (1 min) to 200 °C at 40 °C/min (2 min)
Column 2: 35 °C (2 min) to 60 °C at 100 °C/min (1 min) to 200 °C at 40 °C/min (2 min)