- Start by chilling your material columns. With open sleeved jackets a dry ice/ 99% isopropyl solution will reach -110, and with closed jackets liquid nitrogen is appropriate. Chill the solvent tank at this time as well.
- Once you have reached and are holding desired temp while also maintaining vacuum it’s time to prime the system. We do this by pushing warm vapors from another solvent tank into the system.
- Turn on your recovery pump and open recovery port on your cold tank, allow it to build a bit of pressure. While doing this, remove the cold solvent tank from its chilling bath, place it on your refrigerant scale, then open the liquid port and begin flushing. I do a 10:1 solvent to material.
- Once the solvent has pushed through the material column I let the solute run through my buchner vessel (purchased from open source Steel). I put pro pak distillation packing on top and between the filters to prevent clogging. Freeze with dry ice and iso/etoh for at least one hour. I’ve had clients get good results without dewaxing.
- After allotted time, I open the next valve and allow it to run through the filters into the collection vessel. I recover at 65° to preserve the terps.
- Once it’s low enough open (you want to leave about 1lb of solvent and pour into jars put lid on loose and cryo with dry ice / isopropyl for minimum of 2 days. I do this in an igloo cooler in a deep freeze freezer. During this you’ll see THCa crystals blooming on the walls and bottom of the jars. This is what you want to happen, don’t be alarmed.
- After that let jars sit at room temp for an hour or 2, then tighten the lids all the way and do another couple hours at room temp. (This is only to ensure enough solvent has evaporated so you can tighten the lid)
- Place jars, with lids tight, in vacuum oven at 80-85° with no vacuum, for 14-21 days, sometimes longer depending on the reaction. (For larger diamonds set to 65° this will extend growth time to 3 months even longer. You must be patient for this. I advise doing 85° till youre comfortable.) That’s when your crystals will grow and real separation will happen.
- Once you feel you have achieved proper separation. (You sometimes need to burp after growth has stopped) Open jar and quickly pour terps into smaller jar allow some diamonds to flow in as well. Cap and place back on heat for another week or 2 to ensure precipitation has ended.
- After a week or 2 open terp fraction and begin purging. Leave the oven at 85(this step is not always necessary), pour the terps into a pyrex dish to allow for enough surface area for the solvent to escape. And pull a -15 to -20 vac for 4 days
- While the terp fraction is finishing we advise to put the thca portion in the freezer with capped lid. Place back in oven and purge with the terpene fraction.
The freezing in the jars will force the THCa to crystallize and crash off to the bottom. Then, as it heats up it will dissolve (if you have no pressure it will float to the top leaving seeds everywhere negating the cryo) with pressure it will stay at the bottom and create a clear layer and as the pressure rises the layer gets thinner and more compact until it’s so compact it’s forced to crystallize to get room…
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