This is the ticket
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So I’m not sure if it passed the ethanol test or not. I would say no, but I maybe overly critical. I dissolved 1-2 grams into 1oz of ethanol, 12 hours in the freezer, small but noticeable coagulation in the center. Small, but was easy to spot, even from a few feet away. For sure the cleanest starting material I’ve had.
Went ahead and loaded a cart to see
Eh, I guess I’ll winterize, it’s cloudier then I would like
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If you winterize then you’ll definitely change the terp profile by evaporating the ethanol back out…Unless you’ve got some tricks up your sleeve.
I see nothing wrong with the cart pictured personally.
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Looks like I only got a partial decarb and that’s probably what’s mainly causing the cloudiness in the cart. The oil in the cart isn’t nearly as liquid and runny as it was when I filled it. The sample I pulled yesterday was from refrigerated oil, the oil was very thick and I pulled my sample from the very top surface. Checked my vessel and oil at 70’f ambient temp, dug just below the surface found some thca chunks still, hand stirred and broke them up to try to disperse them more evenly. It has a nice unfiltered honey appearance.
Edit for afternoon update:
Dips pinky in, taste needs more decarb
All along the bottom it’s been vaped, stuff in the middle won’t budge, been sitting upright in my truck all day windows down in the shade, 70’f outside. Too chunky
edit: evening update. got home, the vessel had completely crystalized. I bought a setup from glacier tanks like linked above, but the triclamp on the bottom is the only thing making contact with the hot plate. Not getting good surface contact, because the bottom of the spool is elevated 1/4 from the hot plate. Im relying on the hot plate to heat the tri clamp, which then heats the vessel. My ir thermal sensor cannot read the stainless steel. I’ve ordered a k type thermometer that will arrive tomorrow. Yesterday I ran at 120’c for 3 hours. Today I started at 140’c for 2 hours, but the vessel didnt feel very warm, raised it to 150’c for now, vessel spool is finally getting too hot to touch
debating on buying one of these.
https://www.amazon.com/T-PRO-Sheathed-Thermocouple-0-1000℃-Compensating/dp/B074375LJR/ref=sr_1_95?dchild=1&keywords=k+type+thermometer&qid=1621296995&s=industrial&sr=1-95
I have a lid with two npt fittings on the top, can use one fitting with a cross that has a vacuum gauge, prv and npt/valve. then the other fitting can be this probe, that way I can get a reading on actual oil temps
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You just need a pressure gauge to estimate full liberation of CO2 from THCa.
So are we ok to openly talk about scaling up the decarb (for carts) step now?
I feel like everyone has done it, but no one here talks too much about it.
Would like to discuss SOPs, temps, times, etc. Anyone else want to share besides me?
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We’re just starting up on our cart line now and can share some more data as time goes. we did a few different variations this time, with thca separated from HTE and that thca much longer to fully decarb vs the thca and hte combined that we decarbed.
were using a diamond miner style decarb vessel that i bought parts for off BVV and glacier tanks.
We did 100c for about 24 hours for the thca and hte together.
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Thanks for sharing! We also use something similar to that style chamber. We do the whole extraction together and don’t separate.
We pull a vac and back fill with nitrogen twice prior to applying heat to the chamber. This will reduce/prevent terp degradation and oxidation. Currently we run at 107c until we hit our target PSI. We arrive at that target number by estimating the amount of THCA (70% is our usual assumption in the equation) in the extract and calculating how much CO2 that will be released upon full decarb. Then we apply that volume of CO2 to the volume of the vessel to arrive at our target pressure. This isn’t terribly precise, but it definitely gets you in the ballpark and allows you to know when decarb creeps to a near halt. We generally stop heating once pressure stops creeping more than 0.5psi/30min.
We always leave just a touch of THCA behind, which is great because that’s a decent marker that it isn’t distillate. Residual THCA only seems to become problematic when it is above 5%. And by problematic, I mean decarb continues when oil is re-heated for filling and generates bubbles that screw up filling.
As long as vessel is cooled prior to releasing pressure, any vapor state terps should re-condense. We allow the vessel to cool to 40C prior to releasing pressure. Terp content as a percentage of the oil SHOULD be higher than when you started pending there were no leaks and cool down was allowed to happen. Total weight loss should be 9-10% depending on THCA content, of course.
The oil will need to be “flattened” as well, due to the entrained CO2 still present, but that’s usually accomplished with a quick trip to the vac oven for a gentle purge until you see the carbonation dissipate.
Total process time for 2-2500g is 8 hours give or take.
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Approximately how long are you purging the CO2 (generally speaking, not looking for exact times) and at what temperature?
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It goes in a 50C oven right after pouring from decarb. Takes 30-60 minutes at -22 to -29 depending on the size of the batch and CO2 entrainment. We normally stop the purge if we see frequent large bubbles escaping, as those are thought to be terps. CO2 will generally be small bubbles and come out rather quickly and easily.
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There’s no need to put it in the oven you can just put it in a pot of hot oil with a thermometer in it in order to have temperature control. Also I would use Argan instead of Nitrogen and probably wouldn’t pressurize it the same way you do.
Edit: only after posting my reply my device showed me they were 144 replies to the original post. My reply pertains only to the original post.
As far as winterizing it with minimal terp loss, you can winterize in propane (low boiling temp and thus much easier to purge at lower temperature)
Someone dm’d me and reminded me of the thread where I asked for help calculating these estimated target pressure, so I figured I’d link it.
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Bumping this thread for those of you looking for information on small scale
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Long time lurker here. I finally had to make an account so I could follow up on this. Has anyone been able to continue testing closed vessel with inert atmosphere decarboxylation and been able to get coa’s for comparison?
We are currently looking at different methods of getting our BHO into cartridges and I’ve fallen down this rabbit hole of how to do this without absolutely destroying the terps. With our fresh frozen material, we have been playing around with separating the terps and THCa via diamond miners, melting the diamonds, decarbing, and then re-adding the terp fraction back into the mix (the carts are incredible); however, we continue to have poor separation and the final product is returning with 10%-25% THCa which then leads to an abundance of sugaring once it makes its way into the cartridges. My only lead is that our separation of THCa and terps is insufficient leading to a large concentration of THCa sneaking in with the terp fraction. Long story short, the physical separation via diamond miners has been less than efficient/scalable.
With that being said, we have begun to take a look at utilizing our bulk BHO alongside decarboxylation to get it into cartridges, but our concern is that this will produce dooky carts due to oxidation and terp loss. Based on this thread it seems like people have had success in getting this to work in producing solid BHO carts. Does anyone have any COA’s or anything that could point to a larger amount of terpene preservation - or has this been mostly antidotal based on flavor ect (which I will absolutely take as well).
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Coming up on 1 million out the door…
Always looking for new solutions…
If you haven’t read them yet, I suggest both of these
Did you notice the links below the first post?
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Short answer, yes, it works, and your terp percentage should rise if you do it right and there should be minimal/no oxidation issues.
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Sounds like you need a “spin the shit out of it!” machine.
Do you haz Separation Anxiety (mechanical)
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you can prevent oxidation by doing the decarb in a nitrogen atmosphere. You can reduce (not eliminate) terp loss by doing the decarb at as low of a temperature as possible. This doesn’t require any equipment that can withstand high pressures. In my experience, you can make fire BHO carts using these techniques.
If you want to decarb under pressure, you’ll be looking at significant $s in equipment. Simply because there will be so much pressure built up by CO2 that your equipment will need to be registered pressure vessels (I could be wrong here).
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As long as you do your math correctly, it’s reasonably easy to get off the shelf components in 6" or smaller diameter that will handle the pressure easily and accomplish complete decarb under pressure with no terp loss.
Math is the key, though. And PRVs, just in case your math is wrong.
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