I’ve used the search and found a lot of stuff related to BHO shatter and sugaring problems but couldn’t find anything specific to ethanol.
My process is -80C extraction on frozen, dried material (5% moisture content) rotovap at 30-40C, pour onto parchment paper (no scraping), and into a vac oven pre heated to 93F. After ~1hr at 93F I pull vacuum down to -29.5" Hg. After 24 hours every slab starts sugaring. Has happened with 3 strains so far, two trim, one bud.
Anybody else experience this specifically with ethanol? Any advice?
I’ve only gone for shatter with something that has seen powders once. Filtered ethanolic solution over AC and DE. Neither were prewashed. Will look into prewashing powders, thanks! Even when the oil has seen no powders, still get sugar.
My thoughts of things to try:
Rotovap at higher temp to remove more terps before it goes into the oven, and starting the purge at higher temps in the oven (105-110F) although this seems contradictory to things reported about hotter oven temps causing sugaring. But everything I’ve read is in relation to BHO.
I’d avoid heat for shatter. But you’re likely to get pull and snap that way? The thc-a is what creates the lattice for shatter.
Terps are potentially an issue? Though it seems weird considering what issues most other people have; and that many should’ve made their way into the evapped ethanol.
I’ve read that strains or concentrates high in terps have a higher tendancy to sugar in the oven. I don’t really understand the theory behind why more terps would cause this? Wouldn’t more terps act as a solvent and keep THCa from crystallizing? If anyone can explain they mechanics of this I’d really appreciate it.
I have run my fair share of EHO and poured up to many slabs to count. So when we roto never go higher than 40C. Pour on to parchment but make sure that parchment doesn’t have any creases or wrinkles these are specific areas that can cause crystals to form. Usually we don’t allow the shatter to sit in the oven for a period of time we get right to vac. This part is tricky as I’m sure you have seen but basically muffin on and off till you can pull full vac. Flip every 12 hours. If you see sugar start to happen. Cut it out of the slab and continue on. Some strains don’t make shatter so they are better crumble. If they don’t make either you’re better off pouring up in a Pyrex and going straight for sauce. I would keep a strain book on hand and record which strains do what best. Hope this helps.
You have the temp right about where we keep ours. Once you get past the muffin and it settles down just keep it on full vac. Flip twice a day or more if you want. Usually takes about 4 or 5 days but you can monitor by ethanol content ?
Another failed attempt. Super skunk trim, cured and frozen in -80C freezer extracted with -80C ethanol with 3-5 minute soak. Rotovaped at 35C, poured onto parchment paper, and into warm vac oven set to 89F. Pulled vacuum slowly down to 50 micron (~-28Hg) and held there. Within 24 hours, sugar.
EDIT: 50 torr, not micron
What am I doing wrong? Is this a common problem with shatter attempts made from ethanol? Any suggestions for what to try? So far have tried a range of vac temps, from 89F at low end, to 105F at high end. Sugars every time.
What causes this? Is the cold extraction a problem? Do waxes help stabilize shatter (prevent sugaring), what I’ve read indicates the opposite. Is it a terpene issue? Would rotvaping at a higher temp to boil off more terps help? Would it help to rotovap less so that the oil has more ethanol when I pour onto parchment paper? Right now I roto it down until no more ethanol is visibly condensing and hold there for 20-30 minutes. When it’s poured out it’s pretty thick and requires a heat gun to get it flowing.
Trying to read every related thread on here I can find, but so far have come up short. Specifically not much about this issue from ethanol extractions. Has anyone else had this issue with ethanol? Any help greatly appreciated. Banging my head against the wall here.
how thick are your slabs?
have you had any of the sugaring samples tested for terpenes?
what kind of sugaring, pics please.
-28Hg on a dial gauge, or an actual 50micron? Held there, as in active vac or valved off?
its a phase transition issue, your concentration of dissolved THCa has to be in ideal conditions for it to transition to glass vs crystallize, if your solution viscosity is to low from either heat or solvent/terpenes it will likely crystallize vs glass. basically the idea is to get the solution to proper viscosity with heat to purge the solvent/volatile liquids(terpenes) and then allowing the now higher concentration of THCa to “cool” into a glass vs nucleate. Perhaps your terps are to high, perhaps your vacuum level is not high enough to remove the terpenes if they are in high quantities(not the normal with ethanol or trim, but possible) perhaps your temps are to high for to long. What would happen to the slab if you took it out at 8 or 12 hours before its sugared, and put the slab at room temp or colder for 20 - 60 minutes whats its consistency? Is it runny or tacky/sticky, or harder/bendable almost shatter or something else?
Thank you for the reply, you’ve given me some stuff to think about!
Not too thick. No more than a couple mm, no thicker than a credit card. How does thickness affect propensity to sugar?
I have had 1 tested for terps and it came back as 1.33% total terps, 70% total THC, 5.8% (decarbed THC - not sure if this is higher/lower than normal for these types of waxes?)
Woops, meant 50 torr which is close to -28 on the guage. Always active vacuum with the pump running.
I’ll give this a try. Typically they go into oven at the end of the day and by the time I come back ~15 hours later, they are sugared.
It’s hard for me to believe that terpenes and their effect on viscosity are the issue given that it’s from an ethanol extraction. Maybe too much residual ethanol when I pour onto parchment paper? Kind of doubt that too as I rotovap it for a good while after ethanol stops condensing resulting in a very thick oil.
I doubt it’s related to “too long” as it sugars in under 24 hours, but I will try lower oven temps. Might as well just try 80F. IR thermometer confirms the oven set temp is within 1-2 degrees of actual temp.
Here are some pics. The first few are from my first time pouring a slab that large and I really fucked them up. Poured way too thick and had to scrape off and on to other sheets. Read that scraping can cause sugaring and so subsequent ones were not scraped. Since these pics, I’ve been doing much smaller test slabs to figure out what is going on and on all of those I pour about credit card size or less.
In the past, several months ago, and once this month, I was sucesfull at getting shatter or at least pull and snap on very small test runs. Only difference I can think of between those and these is:
The extractions where I was able to get shatter, were done a while ago and since then maybe my ethanol has absorbed more water and that that may be having an effect? Hydrometer has been ordered and should arrive soon.
The extractions where I was able to get shatter were all longer soaks (30-40 minutes in a -80C freezer) resulting in a darker color (more impurities). More impurities, less likely for THCa to crystallize? But if that’s the case, how are people like LostBiologist and others, able to get such incredible looking shatter from EHO?
The extractions where I was able to get shatter were all rotovaped at 50-55C where as the ones that sugared I rotovaped at 30-35C to preserve color/terps/etc. But plenty of people seem to roto at lower temps and get ethanol shatter, so that doesn’t seem likely.
Tonight, I took some of the same EHO that sugared and am purging it in a heated vac chamber (not my vac oven) to see if that changes anything. Doubt it tho.
These are some old pics of the shatter attempts that were successful:
