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Triple-Phase SPME Arrow vs. Triple-Phase SPME Fiber

ColumnRxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
Standard/SampleResidual solvents #1 (cat.# 34105)
n-Propane, isobutane, n-butane (Emerald Scientific)
Conc.:10 µg/mL
Liner:Topaz 1.8 mm ID straight/SPME inlet liner (cat.# 23280)
Inj. Temp.:280 °C
Oven Temp.:30 °C (hold 6 min) to 85 °C at 15 °C/min (hold 2 min) to 250 °C at 35 °C/min
Carrier GasHe, constant flow
Flow Rate:2 mL/min
DetectorFID @ 320 °C
Make-up Gas Flow Rate:40 mL/min
Make-up Gas Type:N2
Hydrogen flow:45 mL/min
Air flow:450 mL/min
Data Rate:20 Hz
InstrumentAgilent 7890B GC
Sample PreparationA 6 mL sample for residual solvents analysis based on USP <467> was prepared for headspace solid phase microextraction (HS-SPME) as follows:
1. 3 g sodium chloride was weighed into a 20 mL amber headspace vial (cat. # 23086) with screw top cap (cat. # 23090).
2. 6 mL of deionized water was added to the vial.
3. The sample was fortified at 10 µg/mL with the residual solvents, n-propane, isobutane, and n-butane standards.
4. The vial was capped and vortexed at 3000 rpm for 10 seconds, inverted, then vortexed again for 10 seconds at 3000 rpm.
NotesCTC RTC Parameters

Tool: SPME Arrow and SPME fiber
SPME Arrow: Restek PAL SPME Arrow, DVB/C-WR/PDMS, 1.1 mm, 120 μm (cat.# 27875)
SPME Fiber: Restek SPME fiber, DVB/C-WR/PDMS (cat.# 27873.1)
Agitator Speed: 250 rpm
Agitator Temp: 30 °C
Incubation Time: 120 sec
Heatex Stirrer Speed: 1000 rpm
Heatex Stirrer Temp.: 30 °C
Vial Penetration Depth: 35 mm
Extraction Time: 120 sec
Injector Penetration Depth: 50 mm
Desorption Time: 10 sec
Pre-Conditioning: True
Post-Conditioning: False
Conditioning Time: 60 sec
Conditioning Temp.: 250 °C