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

	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)

Oven
Column	Rxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
Standard/Sample	Residual solvents #1 (cat.# 34105)
	n-Propane, isobutane, n-butane (Emerald Scientific)
Diluent:	N,N-Dimethylacetamide
Conc.:	10 µg/mL
Injection	Direct
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 Gas	He, constant flow
Flow Rate:	2 mL/min

Detector	FID @ 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
Instrument	Agilent 7890B GC
Sample Preparation	A 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.
Notes	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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