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

Peaks
1.n-Propane
2.Isobutane
3.n-Butane
4.Methanol
5.n-Pentane
6.Ethanol
7.Diethyl ether
8.Acetone
9.2-Propanol
10.Acetonitrile
11.Methylene chloride
12.n-Hexane
Peaks
13.Ethyl acetate
14.Chloroform
15.Cyclohexane
16.Benzene
17.1,2-Dichlorethane
18.n-Heptane
19.Trichloroethene
20.Toluene
21.m-Xylene
22.p-Xylene
23.o-Xylene
24.N,N-Dimethylacetamide (solvent)
image
GC_GN1204
ColumnRxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
SampleResidual solvents #1 (cat.# 34105)
n-Propane, isobutane, n-butane (Emerald Scientific)
Diluent:N,N-Dimethylacetamide
Conc.:10 µg/mL
InjectionDirect
Liner:Topaz 1.8 mm ID straight/SPME inlet liner (cat.# 23280)
Inj. Temp.:280 °C
Oven
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
NotesA 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.
5. The sample was analyzed using the following CTC RTC parameters.

CTC RTC Parameters
HS-SPME Arrow

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
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