Hello all. I am still waiting on some glassware to arrive, but I will be testing some different methods of terpene collection, prior to ethanol extraction, using a vacuum oven connected to a series of dry ice slurry cold traps, frozen material and nitrogen assist. Testing will include using dried/cured flowers, fresh flowers and dry ice hash. There are tradeoffs with all, as fresh material will have 10x the terpenes but also produce a lot more water-based hydrosol that could dilute and make it more difficult to collect terpenes. After terp collection, I want the material to be almost completely free of moisture in order to do a dry ice cooled 200 proof ethanol extraction. After ethanol distillation and purging, I would combine terpenes, which have been filtered and clarified, with a small amount of HT Pure to create vapable oil.
All that being said, I think the most promising method to prep and process flower material might involve using liquid nitrogen at a few stages to create a hybrid process. Here is what I am thinking:
1.) Use either fresh cut or dried/cured flower, with buds trimmed from main stem and major leaves removed.
2.) Place material in canister with drain holes and dip into liquid nitrogen dewar to fully freeze.
3.) Carefully dump sub-frozen material on prepped stainless 220 (maybe 400-500) micron screen secured to stainless collection pan and quickly dry sieve (crush) all material through screen. The low-profile stainless collection pan will be sitting on a block of dry ice at the bottom of a thermal sink. Screen is removed and any material, not a stem, is added to pan.
4.) Pre-chill vacuum oven with dry ice in stainless container.
5.) Material, which is still in stainless pan on dry ice, is moved to tray in vacuum oven and then sprayed with additional Liquid Nitrogen using a freeze treatment gun/dewar. (EDIT) - OR maybe just pour a larger quantity of LN2 over material.
6.) Oven door is immediately closed and full vacuum is pulled. LN2 will be releasing N2 gas, so no additional N2 backfill is added (I think???).
7.) Experiments Galore - Temp and time ramps are one of the biggest variables in this process to me. It seems that the process of water (within the fresh plant matter or added with distilled h2o or condensation from atmosphere) thawing/evaporating on the trichomes causes the release of terpenes, which with the help of the nitrogen bouncing it along the vacuum, collects in my traps. The heater controls on my AI oven start at 0C, so I can let it rise naturally or begin assisting over this temp. During a single temperature rise cycle, I will also experiment with different terpene collection times. I might collect more often for fresh material on first cycle. To collect, N2 backfill with regulator will be opened lowering vacuum level and drawing terpene gases to collection traps. After set brief collection time, full vacuum will be restored.
8.) After reaching my desired max temperature for the cycle, I will do a full terpene collection and slowly reduce the vacuum to zero with a ball valve on backfill to fresh air. I will then open the oven (and possibly use dry ice to cool it again) and spray the plant material with distilled h2o and then spray it again with liquid nitrogen. Steps 6-7 are then repeated with a higher ending temperature each time, maybe with less collection times as moisture level drops.
9.) Once I feel the material is completely dry, the stainless container of material is removed from oven and placed back on dry ice in thermal sink to cool to -50C. 200 proof ethanol is cooled to -50C and a semi-traditional ethanol extraction, distillation and purge follows.
10.) Terpenes are stored with low head space and then filtered further (still need to read more on this).
11.) Depending on collected terpene volume, all or some is added to a small amount (.05ml-.1ml per gram of shatter) of a stabilizing oil like HT Pure and then mixed with step 9 shatter for vape pens.
Well, this is what I have so far... How will it turn out??? Who the fuck knows, but I really enjoy the process of experimenting and learning. This might seem kind of ghetto to those who to get to play with 5 and 6 figure machines, but this forum (Icmag) has always been about helping the average guy create top shelf! The goal is to use connoisseur grade flowers to create a connoisseur grade extract without breaking the bank (less than $3k) or using Butane. Any input on the process above would be great!!!
WFF
All that being said, I think the most promising method to prep and process flower material might involve using liquid nitrogen at a few stages to create a hybrid process. Here is what I am thinking:
1.) Use either fresh cut or dried/cured flower, with buds trimmed from main stem and major leaves removed.
2.) Place material in canister with drain holes and dip into liquid nitrogen dewar to fully freeze.
3.) Carefully dump sub-frozen material on prepped stainless 220 (maybe 400-500) micron screen secured to stainless collection pan and quickly dry sieve (crush) all material through screen. The low-profile stainless collection pan will be sitting on a block of dry ice at the bottom of a thermal sink. Screen is removed and any material, not a stem, is added to pan.
4.) Pre-chill vacuum oven with dry ice in stainless container.
5.) Material, which is still in stainless pan on dry ice, is moved to tray in vacuum oven and then sprayed with additional Liquid Nitrogen using a freeze treatment gun/dewar. (EDIT) - OR maybe just pour a larger quantity of LN2 over material.
6.) Oven door is immediately closed and full vacuum is pulled. LN2 will be releasing N2 gas, so no additional N2 backfill is added (I think???).
7.) Experiments Galore - Temp and time ramps are one of the biggest variables in this process to me. It seems that the process of water (within the fresh plant matter or added with distilled h2o or condensation from atmosphere) thawing/evaporating on the trichomes causes the release of terpenes, which with the help of the nitrogen bouncing it along the vacuum, collects in my traps. The heater controls on my AI oven start at 0C, so I can let it rise naturally or begin assisting over this temp. During a single temperature rise cycle, I will also experiment with different terpene collection times. I might collect more often for fresh material on first cycle. To collect, N2 backfill with regulator will be opened lowering vacuum level and drawing terpene gases to collection traps. After set brief collection time, full vacuum will be restored.
8.) After reaching my desired max temperature for the cycle, I will do a full terpene collection and slowly reduce the vacuum to zero with a ball valve on backfill to fresh air. I will then open the oven (and possibly use dry ice to cool it again) and spray the plant material with distilled h2o and then spray it again with liquid nitrogen. Steps 6-7 are then repeated with a higher ending temperature each time, maybe with less collection times as moisture level drops.
9.) Once I feel the material is completely dry, the stainless container of material is removed from oven and placed back on dry ice in thermal sink to cool to -50C. 200 proof ethanol is cooled to -50C and a semi-traditional ethanol extraction, distillation and purge follows.
10.) Terpenes are stored with low head space and then filtered further (still need to read more on this).
11.) Depending on collected terpene volume, all or some is added to a small amount (.05ml-.1ml per gram of shatter) of a stabilizing oil like HT Pure and then mixed with step 9 shatter for vape pens.
Well, this is what I have so far... How will it turn out??? Who the fuck knows, but I really enjoy the process of experimenting and learning. This might seem kind of ghetto to those who to get to play with 5 and 6 figure machines, but this forum (Icmag) has always been about helping the average guy create top shelf! The goal is to use connoisseur grade flowers to create a connoisseur grade extract without breaking the bank (less than $3k) or using Butane. Any input on the process above would be great!!!
WFF
