Draft v1.

0 January 2023

HAS Thermal Stability Study – Phase II Testing Plan

1. Individual Solvents

a) Purity test of selected solvents via GC-MS (i.e. direct injection onto GC/MS)
b) Thermal stability evaluation of individual solvents via Py-GC/MS*
c) Check for interactions between DCM and solute – and if necessary we can switch solvents –
e.g. toluene, IPA

2. *Assess sample preparation

Initial assessment of sample preparation for Py-GC/MS when using CBD + solvent (Terp Mixture A)

 Using the same amount of CBD as previously used in neat CBD experiments, compare two
versions of the dilution regime, to see if this has an influence on the pyrolysis, by influencing
the extent of dispersion on the quartz wool.
o Compare e.g., 1 uL of 1 mg/mL CBD vs 5 uL of 0.2 mg/mL CBD). Perform in inert and
also reactive (9% O2) conditions.
o We also want to perform a comparison between quartz wool and an experiment
using a bare pan.

Total sample mass (+ solvent DCM):

Pure solvent mass: ≈ 3μg

Solvent Heating Atmosphere & Comments Heating/pyrolysis

Temperature gas flow time

200 9% O2 and Inert Sample drop 30s?

(carrier gas flow into pre-heated
= 150 mL/min) chamber @
250 9% O2 and Inert designated temp 30s?
(carrier gas flow
= 150 mL/min)
300 9% O2 and Inert 30s?
(carrier gas flow
= 50 and 150
mL/min)
Propylene glycol
(PG)

Propylene
glycol:glycerol
(PG:VG), 70:30
Triethyl citrate
(TEC)
Benzyl alcohol
Terpenes Mixture
A
Draft v1.0 January 2023

Terpene Mixture
B

*All individual solvents will also be evaluated via TGA in identical fashion to previous experiments
(including air vs inert atmosphere) for completeness - COMPLETE

Output of this phase will determine the process for the next phase (cannabinoid formulations)

2. Cannabinoid Formulations

a) Purity test of selected formulations via GC-MS (i.e. direct injection onto GC/MS)
b) Thermal stability evaluation of cannabinoid formulations via Py-GC/MS

Cannabinoid Solvents Cannabinoid Heating Atmospheres Comments

concentration Temperature & pyrolysis
time
CBD, CBG,  PG a) 5% w/w 200, 250, Air (9% Sample drop into
CBC, CBN,  PG:VG 300 C O2/N2) and pre-heated
CBDA  TEC inert (N2), chamber @
 Benzyl b) 50% 150 mL/min, designated temp
Alcohol w/w 30 s pyrolysis
 Terpenes (TBC) time
Mixture A
 Terpene
Mixture B

(add substances in
via DCM)

Other considerations

 Alternative antioxidants
 Distillates/resins/rosins – THC-free distillate (figure out import requirements to Hungary?)