Residual Solvents in Cannabis Concentrates on Rxi-624Sil MS by Headspace–Full Evaporation Technique (HS-FET)

Oven
Column	Rxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
Standard/Sample	Residual solvent mix
Diluent:	Dimethyl sulfoxide (DMSO)
Conc.:	25 ppm (For the HS-FET technique, 10 µL of a 50 µg/mL standard was placed into a 20 mL headspace vial to represent a 25 ppm sample concentration, assuming a 20 mg sample weight.)
Injection	headspace-loop split (split ratio 10:1)
Liner:	Premium 1.0 mm ID straight inlet liner (cat.# 23333.1)
Headspace-Loop
Inj. Port Temp.:	250 °C
Instrument:	Tekmar HT3
Inj. Time:	1.0 min
Transfer Line Temp.:	160 °C
Valve Oven Temp.:	160 °C
Needle Temp.:	140 °C
Sample Temp.:	140 °C
Platen temp equil. time:	1.0 min
Sample Equil. Time:	30.0 min
Vial Pressure:	20 psi
Pressurize Time:	5.0 min
Loop Pressure:	15 psi
Loop Fill Time:	2.0 min
Oven Temp.:	35 °C (hold 1.5 min) to 300 °C at 30 °C/min (hold 2.0 min)
Carrier Gas	He, constant flow
Linear Velocity:	80 cm/sec

Detector	FID @ 320 °C
Make-up Gas Flow Rate:	45 mL/min
Make-up Gas Type:	N₂
Hydrogen flow:	40 mL/min
Air flow:	450 mL/min
Data Rate:	20 Hz
Instrument	Agilent/HP6890 GC
Notes	For qualitative purposes only. The butane used for standard preparation was a mixture of butane and isobutane in an unknown ratio. The concentrations should be considered approximate, but do not exceed 50 ppm for any component.

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