- SDS Sheets: Available upon request on all chemicals used in this process.
- PPE: The following should be worn by all lab personnel during Ethanol extraction:
- Splash Goggle
- Lab Coat
- Select DV with a maximum capacity of at least twice the volume of oleoresin used, add magnet Stir Bar, and record the Tared weight of DV.
- A stainless-steel vessel (Bain Marie) is recommended due to its durability and higher heat transfer coefficient, however a glass beaker will also work well.
- Fill up to one-half of the total volume of the DV with extracted oleoresin. Record Oleoresin weight with DV tare weight subtracted.
- Using a Controllable Heat Source (Hot Plate, Induction Cooktop), select your appropriate temperature based on time allotted.
- Decarboxylation Times and Temperatures (Approximately while data supports these times, original composition of Oil can change time required. Continue operation until production of small semi-table CO2 bubble ceases).
- 60 minutes at 130 ˚C
- 180 minutes at 110 ˚C
*Temperatures and times for decarboxylation are reliant upon a thin film of reactant, thick solutions allow for such less efficient and heat distribution and gas exchange, so thicker solutions will need more time to Decarboxylate fully.
- Set Stir function (magnetic or overhead stirrer) at 240-1500 RPM to allow proper gas exchange.
*Lack of stirred agitation will result in boil over.
- If a layer of tiny bubbles grows on top of the Decarboxylation, use a stainless steel or glass stir rod to break up layer.
* Allow Decarboxylation to continue until production of small semi-stable CO2 bubble ceases.
If using Vacuum: Initiate vacuum to system by turning on Vacuum Pump. If -50˚C or lower Cold Trap cooling is possible, full vacuum (2-20mmhg) is suitable. If these low depths of temperatures cannot be reached, regulate Vacuum at 200-350 mmhg, as to ensure full retention of fragrant compounds.
- Initiate heating of the Mantle until Oleoresin temperature reaches 75˚C, then initiate magnetic stirrer to 100-250rpm.
- Raise mantle temperature to 100˚C. Wait 15 minutes or until total oleoresin is liquid and flowing with the stir bar.
Note: If using Vacuum, starting with vacuum pulled on the system, a ramp from 50-75-100˚C is suitable, and will help mitigate any foaming or bumping up the fractional distillation column.
- Once oleoresin in liquid and flowing with stir bar, raise Stirrer RPM slowly until maximum RPM is achieved. Fast Stir bar revolutions are important as a vortex is needed to break up the semi-table CO2 bubbles that form as a foam on top of the oleoresin. This is especially necessary in non-vacuum operations.
- Raise Mantle temperature to 125˚C after 20 minutes to allow for a gentler distillation of the lower molecular weight volatiles, preventing degradation of the Essential Oil.
- Continue Decarboxylation until cessation of small semi-stable CO2 bubble production. This marks the end of the Decarboxylation.
- Once Decarboxylation is finished, turn off heat to the mantle, and allow oleoresin temperature to lower to below 70˚C.
- If Vacuum is used, turn Vacuum pump off and open system to atmosphere.
- Disassemble system, clean off any used Joint Grease, and clean each piece of glassware except the Oil-Water Separator.
- Remove Hydrosol from Oil-Water Separator and collect in a sealable container.
- In a Cold Trap was utilized, remove Cold Trap from coolant bath, wipe dry with a towel of cloth.
- Remove contents of cold trap and add it to Oil-Water Separator, Rinse Cold Trap with distilled water of hydrosol and add that to the Oil-Water Separator as well.
- Drain off Hydrosol, collect into Hydrosol container.
- Drain off Essential Oil into suitable container. Place in freeze for 24 hours to freeze any lasting H2O in the oil. Pour essential oil into secondary suitable container.