Ethanol Muffin Under Vacuum - What are my options from here?

Hash and Stuff Pre/Post-Processing
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Heated vac oven set to 142F, dial on chamber reading just below -30inHG.
So right before these pictures were taken, I whipped up the extract in an attempt to help residual ethanol escape. Prior to this, it had been sitting on my dresser top for maybe 5 days or so possibly a week. Even prior to that I had the extract under vacuum for 3 or so days at roughly 100F. I did the extraction at around -50C or so, ran thru AC and T5 a few times and distilled out most of the ethanol at around 44-45C, as my vacuum is not as strong as I would like.

So my question is, is the muffing in my extract just excess oxygen from whipping it? Ive been attempting to create sugar wax with ethanol but so far am not having any success in that field. I have only been able to make pull and snap so far in my attempts to make sugar.

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If you want to get any nucleation (sugaring) out of ethanol extracts I’ve found like 4 ways to make it happen, thoughI pull terpenes off my material prior to introducing etoh so my processes may not be super helpful for you, but might point you in the right direction. I’ll also note that working with the freshest material you have access to will make a difference in terms of how long it will take to get to the formation sizes you want.

Number one, and by far the easiest, is leave residual ethanol in your extract after the roto or whatever evaporating system you’re using. (Sounds like you’re already there with your current approach) While that mixture is still at the temp you were evaporating at, pour it into a mason jar, slap a lid on (tight), and leave it in a cabinet at room temp (22-23C) for a couple days. I tried not to disturb the samples I was testing this on but didn’t notice much difference in terms of clarity or geometry as they progressed. After a couple days you can tell if it worked. You’ll either see nucleation beginning in the body of the extract or a translucent extract. Like I said, my material is deterped before I pull cannabinoids off, so I’m not sure what this process is going to do to your terpene profile, or how a terpene laden primary extract will behave.

2 is sometimes I can get my cannabinoid extract to crystallize or budder up in the rotovap around 87-89C. Not consistent, and seems to be specific to a couple chemovars we work with.

3 is remove all the ethanol you can, jar and lid tightly, and use a bead bath (you can make one with a hot plate, a stainless container, and metal bbs), oil bath, whatever to apply consistent and regular heat at 65-70C for a couple hours. The heat should make your extract viscid enough to let the thc-a move enough to start forming nuclei. If you’re not sure you have all your solvent out don’t do this because you will blow something up.

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I’ve been trying to reproduce this as well. Were you able to consistently replicate the sugaring with your mason jar approach?

I tried a few times but couldn’t get anything to grow. I have seen it happen in perfect storm scenarios but I have been unable to successfully reproduce it to the same scale.

Every time it’s happened for me thus far has been with super saturated ethanol extract from de-terp’d, high potency, fresh material. When I try to recreate the conditions by removing the optimum amount of solvent at low temperatures instead of supersaturating the extraction, it seems to fail. At the minimum, I can usually produce a glassy, semi-solid syrupy solution, but never a crude sugar.

Do you have any guess at the optimum residual ethanol level for fast nucleation?

In my experience, 40% seems high, and 5% low.

My next experiments are going to involve seeding using THCa isolate, but Im still working on the DOE.
Any tips for a mason jar setup would be much appreciated :slight_smile:

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Rather I should say, are you ensuring your material is not loaded with fats from long residency at -50 or warmer temps?

I haven’t had first hand experience with nucleation and ethanol extracted substances, but I would imagine the principles of getting rosin to nucleate are similar - whether it happening on its own while being pressed or forcing it afterwards with heat + time

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Out of curiosity (and out of the blue since this post is 20 days old), what process are you using to strip terps?

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My thoughts went the same way yours did, and I say seed that bitch! You could always use another solvent; pentane is the first one that comes to mind.

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Not winterized, but extracted at temps below -50, using spent material from CO2 terp extraction. Pentane or other hydrocarbons would be great, but I want to see if I can isolate THCa from ethanol crude without additional solvents.

I’m going to sprinkle in some THCa isolate and work on maintaining cold extraction temps, and use room temperature solvent removal. Stop removing solvent at a point where it remains viscous and flowy (10-20% by mass?) and then place in a pyrex dish (one inch volume height) with the bottom etched up under cold vac and purge for a week or two. Monitor the growth without disturbing.

I’m also playing with the idea of using sudden bursts of ultrasound under similar parameters, but I need to be way smarter before I attempt that. And I have tried doing this under N2 pressure with some success, although it was too slow and with too low a yield for my liking.

Any tips to add onto that setup?

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The muffining you are seeing is the crude decarbing. If you watch your processes closely enough, you will see the difference between solvent bubbles and those produced through decarbing. Solvent bubbles are big, while decarb bubbles are really small.

The biggest reason you are likely not getting sugar to form (aside from some process issues others seem to be trying to help with) is because you are decarbing. THC doesn’t like to crystalize; THC-A does. If you decarb, it doesn’t want to crystalize.

Some reading to help:

Lots of people have been talking about how to do this for a while. There’s some good info on the site. Also, sorry it took 20 days to notice this @Brukang.

Edit: and @bogue, the above links may help you too. There were a ton more results my 30 second search produced as well.

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My primary extraction is three step LCO2/CXE, pulling terps off material is part of the process

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Many thanks :pray:

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Hey Akoyeh,

I did the search as well, thank you for posting. Maybe this wasn’t the best thread to start the convo up in and I might have posted before reading enough but since I’m already here…

Decarbing is not the issue, I test for that.

I had spontaneous crash out happen with neglect tek in under a week at high yields and I am trying to reproduce it.

Essentially, I left crude ethanol extract in solvent solution for a weekend and came back to a bed of crude crystals sugaring into a paste. I decanted and kept the paste which I was able to filter and isolate THCa very easily at high purities, with minimal waste and usable byproducts.

Typically my solvent removal leaves a dry extract, but this neglect tek was an unknown amount (probably between 20-40%) that was left in process.

I am playing with recreating that neglect tek with trials but as things fail, I am starting to see that regardless of the input potency and process conditions, the strain dictates whether it will crash out or not. I pulled low BP terps off the input cannabis for this last experiment, but the terps that remain might be the issue.

I had read some of @THChemist posts and see that he has a better understanding of how the terps could both hinder and help crystallization, and I believe that to be true in this case. I’m working on quantifying the terps in my first neglect tek so I can reproduce them again, but in the mean time, I’m throwing every trick I have at it:

Cold extraction (lower than -60) with 95% etoh (I am ordering 100% to try as well)
Input biomass dewatered and stripped of terps (less than 5% moisture) and greater than 20% THCa
High potency supersaturated crude extract with 1micron filtration (bud to solvent ratio at 3:10)
Cold ethanol removal (room temp in a rotovap, max vac)
Add ethanol back at varying quantities to know exact ratio
Periodic evaporation of solvent to the vessel (burping once a day?)
Pressurized vessel (10psi)
Etched glass surfaces
Seeded solution
Initial vibration of the solution
Cold temperature cycling (once a day down to -60C)

If there’s any other tips, I am all ears, and would greatly appreciate any advice. Thanks :slight_smile:

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How are you testing for % decarbed? It still really looks a lot like decarbing to me. While the heat being applied isn’t super high, it is still enough to initiate the decarb process. Even time spent on the rotovap and method of feeding vs loading can make a big difference. Not saying you’re wrong, by any stretch of the imagination. I’m just curious.

Haven’t played much with (THC-A) ethanol crystals, so I don’t have a lot of advice in that regard. I can tell you, though, that I’m not fond of 200 proof for extraction. 190 is my preference, and keeping your filtration cold, especially if utilizing the T5/AC combo, you’ll have far better results.

I am also curious as to why you are terp stripping prior to extraction. Terpenes act as a cosolvent and seem to assist in the process (at least as I see it). Are you capturing and reintroducing them? Unless it’s going to distillate or the terps are captured and reintroduced, I am having trouble seeing why this is part of your process.

And you starting this thread is totally the right place. You should have no worries in that regard.

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Testing is HPLC in a lab (and verified with preparative GC) and I decarb a sample of dry extract with pre and post weights to roughly verify.

Do you know a decarb ratio/percentage that prevents crystallization? The last input biomass I used was 30.7% THCa and 0.8% THC.

Also, the terps are pulled for reintroduction later, but in this case I am doing it to remove moisture further without decarb, increase potency and reduce impurities (terpenes that do no dissolve THCa). Only some terps are cosolvents, and in small amounts they can act as impurities that hinder crystal nucleation (I think).

Honestly, I’m not sure if terps, help or hinder, but without them I should be able to crystalize in ethanol, and with them I am not so sure (probably depends on their mass % and the specific blend). So I went with that approach to try and standardize the process without terps before adding (or not removing).

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I don’t have a specific number off the top of my head, but because THC-A likes to crystalize and THC does not, the more THC present, the less there is to crystalize.

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the terpenes absolutely assist in crystallization. You need a solvent in order to allow the solute (THCA) to move around and crystallize. 60-70% THCA in your extract should be saturated enough to crash out.

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Thanks THCehmist, is that 60-70% dry or with solvent?

When my neglect tek ended up producing crystals, I think the density separation over a short period of time allowed concentrate to accumulate at the bottom of the container and create pseudo-partitions which formed a transitionary-metastable-zone. As the extract fell from the solvent dense tops through to the extract dense bottoms, the in-between phases allowed the extract hit a point of supersaturation with optimum viscosity for the ideal amount of time that enabled crash out, and then accumulation at the bottom.

It’s just a thought, but if that’s the case with my neglect tek, my next trials (with adding limited solvent back to dry extract) do not focus on optimizing this density separation approach… I’m not really sure what direction to take it in and it feels more and more like I’m lobbing darts with a blindfold on and hoping for a bullseye.

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That may be true. I think you need just enough solvent to allow movement if your looking for a sugar, more if you’re looking for larger formations.

Something to experiment with may be resolvating in terpenes as opposed to ethanol. then using a little heat to promote crystallization.

I just always keep thinking back to rosin jams and sauces. There is no other solvent present other than the terpenes. Ive seen some impressive formations come from solventless extracts.