Why won't my dewaxed bho slabs stabilize?

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cosmicharlie

Active Member
I am running a close loop extractor w/ a dewax chamber and 8 micron filter. My slabs will not stabilize even when left in the oven for weeks at low temp 85f up to 125f. There shouldn't be a need to go any hotter in a vac oven. I maintain temps during extraction well below 100f and pressure no lower than -28 in hg. I have tried paper thin pours and multiple strains, nothing will stabilize enough to even flip.

I can't find any really clear or complete information on exactly what has to happen on a molecular level for oil to stabilize and shatter at room temps. Why are some strains great for shatter and others not?

What about winterizing w/ pharma alcohol? How can an oil stabilize if you remove all the fats and lipids?

Chemist help me!!!!
 
Fadedawg

Fadedawg

Well-Known Member
What are you extracting, how is it prepared, what is your process?

How unstable is your product?

Shatter is in carboxylic acid state. Decarboxylation, monoterpene enrichment, and residual solvent will make it looser. High levels of plant waxes will make it softer and pliable.
 
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cosmicharlie

Active Member
I have run flower and trim not much prep for the material I have run really dry sugar leaf moister content probably 1-2% and flower as well but there is no difference in the color or viscosity of the oil. I don't pack my material sleeve very tight and use about 4 lbs of N butane per pound of material. I vac the entire system to about -26 in Hg. After the butane is through the sleeve it sits in a dewax chamber chilled with dry ice for at least 2 hours. The super chilled butane is then pulled through a 8 micron filter and into the collection tank. I transfer the butane out of the collection tank and usually I don't even have to use a warm water bath because of the low temps you can reach with dry ice.

I have poured slabs that have almost no butane left and poured some slabs that have a little bit more butane to try and get the slab thinner but the results are the same super sticky oil. Even after the slabs have been in the vac oven for weeks they are still to sticky to even flip. I do vac purge a few times in the oven -28 in hg at room temp before I turn on the heat starting at 85f and over days slowly raise the temps until the slab looks like a shatter should, that is a beautiful color and very glassy but very sappy. I don't take the temps above 125f but low or high temps don't seem to make a difference. I am afraid to go above 125f for fear to decarboxylation.

I know there are a shit load of monos because the oil is super tasty. I was going to try to winterize with some pharma alcohol but I don't know if winterization removes the mono terps. I don't quite understand how winterizing with alcohol would get more wax out if the butane solution has already been winterized and filtered during the extraction.

Do I need to be drying the material before the extraction to remove more of the monos from the plant matter before the extraction?
 
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alwayslearning777

alwayslearning777

Well-Known Member
I drove myself crazy, i had a similar problem, id gotten some trim to blow for a buddy and it just didnt harden up, i tried it my way and two other ways just playing with it and same result a little goopy, i finaly harvest and blow mine and no issues came out great and workable, went back to his trim same process and his still came out a bit tacky ... this probably doesnt help much but from what i found the strain has to have some sort of effect , sry cant really help ya but figured id share what ive learned
 
Twitch

Twitch

Well-Known Member
Some nutes like terpnator make it more gooey. I have a client I run for and his gdp comes out gooey and I got my gdp cut from him and mine comes out shatter. Also what temps atr you runnig and does your cls have adry ice sleeve.
 
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cosmicharlie

Active Member
Twitch said:
Some nutes like terpnator make it more gooey. I have a client I run for and his gdp comes out gooey and I got my gdp cut from him and mine comes out shatter. Also what temps atr you runnig and does your cls have adry ice sleeve.
Click to expand...

I have a dry ice sleeve on the column usually let it chill for 2 hours before filtering. I have done runs where the temps during the entire process were under 70f.
 
C

cosmicharlie

Active Member
alwayslearning777 said:
I drove myself crazy, i had a similar problem, id gotten some trim to blow for a buddy and it just didnt harden up, i tried it my way and two other ways just playing with it and same result a little goopy, i finaly harvest and blow mine and no issues came out great and workable, went back to his trim same process and his still came out a bit tacky ... this probably doesnt help much but from what i found the strain has to have some sort of effect , sry cant really help ya but figured id share what ive learned
Click to expand...
So what is your process in preparing your trim? How fresh and how dry?
 
Fadedawg

Fadedawg

Well-Known Member
cosmicharlie said:
I have run flower and trim not much prep for the material I have run really dry sugar leaf moister content probably 1-2% and flower as well but there is no difference in the color or viscosity of the oil.
Have you actually measured it, or is that an estimate? When you get to that low a moisture content, you are also typically low on monoterpenes as well, plus the material is frangible.
I don't pack my material sleeve very tight and use about 4 lbs of N butane per pound of material.

I typically figure three volumes for most material, and at 4.1 grams per cubic inch for ground material, that would take about 111 cubic inches, which in butane would weigh about 2.4 lbs, so three volumes is about 7.2 lbs. We do run subzero butane, which slows down extraction rates, so it isn't apples to apples.

I vac the entire system to about -26 in Hg. After the butane is through the sleeve it sits in a dewax chamber chilled with dry ice for at least 2 hours. The super chilled butane is then pulled through a 8 micron filter and into the collection tank. I transfer the butane out of the collection tank and usually I don't even have to use a warm water bath because of the low temps you can reach with dry ice.

What kind of n-Butane and has it been pre-distilled to remove mystery oil? How long has it been in the tank and when was the last time you purged it of water?

I have poured slabs that have almost no butane left and poured some slabs that have a little bit more butane to try and get the slab thinner but the results are the same super sticky oil. Even after the slabs have been in the vac oven for weeks they are still to sticky to even flip. I do vac purge a few times in the oven -28 in hg at room temp before I turn on the heat starting at 85f and over days slowly raise the temps until the slab looks like a shatter should, that is a beautiful color and very glassy but very sappy. I don't take the temps above 125f but low or high temps don't seem to make a difference. I am afraid to go above 125f for fear to decarboxylation.

I have better luck heating the thin film until its fully molten, usually between 110F and 120F, and then pulling a vacuum until it reacts with a flurry of boiling, then holding at that level until it stops, then increasing vacuum until it starts, repeat, etc, and then flip when it stops reacting at -29.5" Hg.

I know there are a shit load of monos because the oil is super tasty. I was going to try to winterize with some pharma alcohol but I don't know if winterization removes the mono terps. I don't quite understand how winterizing with alcohol would get more wax out if the butane solution has already been winterized and filtered during the extraction.

Single solvent dewaxing may reduce plant wax content, but it isn't as effective as using a solvent with a higher dielectric constant, so that the wax is even less soluble.

Do I need to be drying the material before the extraction to remove more of the monos from the plant matter before the extraction?
Click to expand...
Maybe more moisture left in the plant material, but subzero butane for extraction.
 
Twitch

Twitch

Well-Known Member
With iso and dry ice you can get the sleeve to -70. Dry ice is generally -70 to -90, I don't feel like googleing it to confirm. That mixed with the iso will help with thermal transfer and get it cold quick. Those temps will help lock up a lot of stuff and the moisture. GW you would know the facts of that off the top of your head.

cosmicharlie said:
So what is your process in preparing your trim? How fresh and how dry?
Click to expand...
Bone dry pack in vac sealed bags place in freezer then the next day crush to a dust then it is ready to start the processing. I have all my clients dry out the material and store it in a freezer till they can get it to the shop to be processed.
 
Fadedawg

Fadedawg

Well-Known Member
Twitch said:
With iso and dry ice you can get the sleeve to -70. Dry ice is generally -70 to -90, I don't feel like googleing it to confirm. That mixed with the iso will help with thermal transfer and get it cold quick. Those temps will help lock up a lot of stuff and the moisture. GW you would know the facts of that off the top of your head.


Bone dry pack in vac sealed bags place in freezer then the next day crush to a dust then it is ready to start the processing. I have all my clients dry out the material and store it in a freezer till they can get it to the shop to be processed.
Click to expand...
Dry ice is -79C/109F, so possible to hit -70/90F with bath.
 
alwayslearning777

alwayslearning777

Well-Known Member
cosmicharlie said:
So what is your process in preparing your trim? How fresh and how dry?
Click to expand...
Hey sorry for delayed responce, ive only got my phone right now so its kinda sucky to give a couple page response ...
In prepairing my trim i always first trim everything wet, i hate trimming after its started to dry, i feel like u can get a nicer tigher trim when its wet, then leave it all out on some silk screens, turning it as needed, let it dry untill it crumbles and then pack the tube so it all breaks up as its going in the tube. Then i leave the tube in the freezer for a few hours. Id say a week or a little more i leave it in my cabinet in the dark, part of the reason i let it get so dry is a collect all the dry sieve, as im packing it in the tube over the silk screen i get a decent amount of trics that fall threw the screen
 
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cosmicharlie

Active Member
Subzero butane meaning you chill the butane before the extraction? What about higher temps in the oven with a lower pressure? Is -29.5 a magic number when using lower temps (125f)? If you were to vac at -25 hg what is the temp that decarbing starts?

I will give you an update on my next round. Thanks guys
 
FlowerPower88

FlowerPower88

Well-Known Member
I had a small batch of bho that would not stabilize with a week in the vacuum oven at 96F, extracted with BVV’s triblend in a pressurized closed column with a dewaxing sleeve kept topped right up with palletize s dry ice and 99% iso. This batch is/was extremely strong smelling, citrusy. The strain is Cali-O. Do you think it could be just really terpene rich and that’s stopping it from stabilizing?
 
Fadedawg

Fadedawg

Well-Known Member
FlowerPower88 said:
I had a small batch of bho that would not stabilize with a week in the vacuum oven at 96F, extracted with BVV’s triblend in a pressurized closed column with a dewaxing sleeve kept topped right up with palletize s dry ice and 99% iso. This batch is/was extremely strong smelling, citrusy. The strain is Cali-O. Do you think it could be just really terpene rich and that’s stopping it from stabilizing?
Click to expand...
What are you calling stabilizing? What consistency is it now and what do you covet?
 
FlowerPower88

FlowerPower88

Well-Known Member
I would like it to hold that Swiss cheese like consistency of shatter, and it is close, but just slightly too viscous and goes to a solid thin sheet of bendy pull and snappy type stuff, but I am at the same temp I usually am, I’m in a different, much more scientific vacuum oven though, as opposed to an acrylic dome chamber with heat plate.
 
Fadedawg

Fadedawg

Well-Known Member
Do I understand that you wish it to be more brittle versus pull and snap?

Retained terpenes and decarboxylation will both lower the viscosity. What temperature and vacuum level are you running?
 
FlowerPower88

FlowerPower88

Well-Known Member
Fadedawg said:
Do I understand that you wish it to be more brittle versus pull and snap?

Retained terpenes and decarboxylation will both lower the viscosity. What temperature and vacuum level are you running?
Click to expand...
Just under -14.5 psi for vacuum and 96F for temp
 
Fadedawg

Fadedawg

Well-Known Member
I suggest using a micron or inch/hg gauge for more accuracy, but you are in the ballpark. How fast can you pull down? What size oven do you have and what size pump?

How old is your trim? If naturally partially carboxylated, or high in terpenes, it will remain soft.

Running it an extended period, even at 96F, will also make it soft.

Wax can soften it as well. What temperature did you extract at? Do you have inline dewax?

I've had good results placing a thin layer in a preheated vacuum oven, allowing it to come up to temperature, and then pulling the vacuum. When the bubbling action becomes too intense, I hold the vacuum at its current level until it calms down, and then resume pumping until I reach 10,000 microns or -29.5in/Hg without large solvent bubbles.

The small fizzy bubbles are CO2 from decarboxylation, so stop before the big bubbles turn to small fizzy ones.

For what it's worth, I prefer pull and snap to brittle shatter, because it can retain more terpenes and is easier to dab because it doesn't shoot fragments across the room when I'm trying to detach a piece for dabbing.
 
FlowerPower88

FlowerPower88

Well-Known Member
I guess it’s more like 14.6-14.7. That’s just the gauge in my oven, I think it also gives bar for a unit as well, which is also way to small a spectrum for accurate measurements, but I mostly just watch the extract, the little pinhead sized bubbles start to develop around -11.5-12 psi and then by the time my pump has achieved as close to vacuum as it’s gonna get the bubbles are starting to break the surface, and a few minutes later it’s purging like a MF’er.

the oven is 0.9 cubic feet and the pump is a 5cfm Robinaire, and it takes maybe 90 seconds to pull down (I am terrible with judging time:dunce:).

this was outdoor nug run, but it was very potent smelling, the bud was probably 5-6 months old though. I was kind of thinking it was the terps keeping it a little more gooey, but the thing that was odd, was I never reached a spot in the purge where the activity slowed down. I would let it purge under vacuum, and then the action would slow down after 12-18 hours on that side, I would take it out, set it in the freezer for 5 seconds, and then flip it. Let it sit in the oven for awhile to get back up to temp, then pull vacuum once more. And it would start right back up…my oven has a 99 hr timer on it, and I ran it all the way through, then I ran it again, from 99 down to 18 or something, it bubbled right til the end. Was I purging terps? I was under the impression that terps didn’t start boiling off even under vacuum until the low 100’s.

I do have an inline dewax, I was from -80-(-150), my temp gun doesnt go past -50, but I was using dry ice and 99.9% iso slurry.

yeah and to be honest I’m not ever mad at pull and snap, the consistency is nicer to handle for sure, but I have been really trying to get that stereotypical Swiss cheese bho shatter look of a slab, more so just to understand what I am doing and how that is translating to the extract, so that I can in the future, do what I or somebody else would like me to at will.

thank you for your time, I will try the partial vacuum gradually increasing as the purge regulates next time. I have always just had the dewaxed solvent/solute in my Pyrex from my column, then I put that in a warm water bath while my vacuum oven gets to temp. Then when the solvent/solute mixture approaches the desired oven temp, I put it into the oven and wait for maybe 3-5 minutes to make sure it’s at temp, then I pull vacuum. This is the first time I have used this oven, and it seems to be fantastic…but it is also the first time this has really happened as well, which is what makes me unsure of the whole thing.

guess I’ll just have to set up another run. Lol
 
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