Making absolute

KLITE

KLITE

Well-Known Member
Hi all

After coming across the best absolute shatter ive come across ive decided to give smoking absolute daily instead of bho.

The person who made it claims the best results he gets are from mixing hot ethanol (around 50C) and mixing it with the butane solution inside the collection chamber of the closed loop after etraction. He says that way for sure all the butane evaporates and that the reaction is VIOLENT! (i suppose so that the minus 20 butane and the plus 50 ethanol might combine and make a temp of ie 10c) He also does not use a vacuum oven after frwwzing and filtering simply put it on a pyrex with lab hot plate underneath at 70C gets a layer as thin as possible by not putting too much of the ethanol solution on the pyrex waits til ethanol is purged and scrape. Finished

Id appreciate any input as i try and devise a way of making absolute. What does that method seem like to you? I like the idea of not using vacuum as from personal experience i feel a short period of high temperature will lose less terpenes than a longer period at moderate temperature under low pressure, got no evidence to support it tho just what ive personally concluded (maybe im wrong).

thanks
 
Fadedawg

Fadedawg

Well-Known Member
When we make Absolute, we typically wash the oil out of the Terpenator pot with hot ethanol. Cold will work, hot is faster.

We then freeze at 0F for about 48 hours, and vacuum filter.

We recover most of the alcohol using a rotary evaporator, but originally put the alcohol out in a shallow casserole dish to evaporate, under a layer of cheese cloth to keep dust out. We sat that dish on about a 135F heat mat.

High heat will not only lose terpenes, but change their form, so vacuum is actually your friend. We run about -28" Hg for ethanol.

That brings us to level of purge. Ethanol is a GRAS (Generally Regarded As Safe) solvent, so some residual isn't unhealthy, even if its unwanted. Some folks like the sweet taste it imparts at low levels.
 
chemphlegm

chemphlegm

Well-Known Member
"He says that way for sure all the butane evaporates"

he should already know when its complete? in a closed loop system he knows how much butane went in,
dont stop recovery till the same comes out? = complete?
 
KLITE

KLITE

Well-Known Member
When we make Absolute, we typically wash the oil out of the Terpenator pot with hot ethanol. Cold will work, hot is faster.
We then freeze at 0F for about 48 hours, and vacuum filter.

We recover most of the alcohol using a rotary evaporator, but originally put the alcohol out in a shallow casserole dish to evaporate, under a layer of cheese cloth to keep dust out. We sat that dish on about a 135F heat mat.

High heat will not only lose terpenes, but change their form, so vacuum is actually your friend. We run about -28" Hg for ethanol.

That brings us to level of purge. Ethanol is a GRAS (Generally Regarded As Safe) solvent, so some residual isn't unhealthy, even if its unwanted. Some folks like the sweet taste it imparts at low levels.
Click to expand...
Thanks fade, how long would you vac purge the ethanol? Will you that at room temp or higher?


I did a little trial today and i have to say i was impressed how much impurities were present in 4g of oil :( I definitely will stop dabing unwinterized oil on a daily basis....

Im hoping it will come out brittle as can be, i used two coffee filters and let the filtered ethanol sit in freezer 4 h to see if anything clouded up and nothing. I suppose it will be just a temp play to get the desired consistency.
 
KLITE

KLITE

Well-Known Member
he should already know when its complete? in a closed loop system he knows how much butane went in,
dont stop recovery till the same comes out? = complete?
Click to expand...
Not the residual amounts trapped by the oil. I always lose around 100g of gas (abt half a can) with every run.

By mixing another solvent at a higher temperature with butane that has a boiling point of minus 1 C and homogenizing it, for sure butane will boil out of the solution.

To be honest i plan on dabbing as long as i possibly can, even if my extracts came out at 90% cannabinoids (which im sure i wouldnt test over 80 on my best ones) i think its still worthwhile polishing it off as much as you can.Fairenough you might lose terpenes too but you get a so many impurities out that will eventually coat your lungs.
 
Fadedawg

Fadedawg

Well-Known Member
KLITE said:
Thanks fade, how long would you vac purge the ethanol? Will you that at room temp or higher?


I did a little trial today and i have to say i was impressed how much impurities were present in 4g of oil :( I definitely will stop dabing unwinterized oil on a daily basis....

Im hoping it will come out brittle as can be, i used two coffee filters and let the filtered ethanol sit in freezer 4 h to see if anything clouded up and nothing. I suppose it will be just a temp play to get the desired consistency.
Click to expand...
We currently use a rotary evaporator to remove the alcohol. https://skunkpharmresearch.com/evaluation-of-heidolph-instruments-hei-vap-precision-ml-g3/

When I used a casserole dish, I put it on about a 135F heat mat and covered with a towel. It usually takes overnight to remove most of it and a couple days to harden up.
 
KLITE

KLITE

Well-Known Member
We currently use a rotary evaporator to remove the alcohol. https://skunkpharmresearch.com/evaluation-of-heidolph-instruments-hei-vap-precision-ml-g3/

When I used a casserole dish, I put it on about a 135F heat mat and covered with a towel. It usually takes overnight to remove most of it and a couple days to harden up.
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Oh ci was under the impression you would cold boil the ethanol off. Why not that way? I did a lil try batch and vacced at 30C and in abt 12 hours no reaction was going on.

Out of curiosity, in the roto vap how do you then remove the en product from vessel? Is it viscous enough or will it be hard?

Thanks

EDIT:

Also how safe is it to have residual amounts of ethanol in your extract, as you claim somepeople like the residual taste. Ive read a couple of things claiming inhalation of ethanol vapor can in the long run have adverse effects on the ocular nerve. Id just like to hear what you know.

I have no way of telling how little residual i have in my bho, i purge at low temps (33 or 35 max) for 5 days or so and flip... but i definetly can tell the little test run i made smokes waaaaaay smoother and cleaner than my bho. I suppose partly due to a good removal of waxes etc but it also made e think perhaps my bho doesnt come out as purged as i thought :(
 
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Fadedawg

Fadedawg

Well-Known Member
You can cold boil ethanol off. It boils at around 72F at -27.6".

We chase it out of the boiling flask with a heat gun. I've also decanted early, while it would still pour without leaving a heavy film, and finished it off in the vacuum oven, in a casserole dish with a pane of glass over the top to contain bumps.

I've read that methanol attacks the optic nerve and that isopropyl attacks the auditory nerves, but not that ethanol vapors damaged them when ingested through the lungs.

It also doesn't logically follow, given that we can drink the stuff in larger amounts and not have the same problem.

The ports of entry into the bloodstream of the human body is oral, topical, suppositories, and the lungs. Once in the bloodstream they circulate to places like the optic and auditory nerves, but the auditory nerves are not directly accessible from the lungs otherwise.

My first reaction, without data to the contrary, is that it is propaganda.

Yeah, winterized is way smoother, both from the removal of the C-30 plant waxes, but by also reducing the C-10 monoterpenes as well, some of which are expectorants.

The scramble for flavor and aroma comes at a cost to smoothness.............
 

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Fadedawg

Fadedawg

Well-Known Member
As an aside, we once did a ethanol/nitrous oxide extraction, and when we depressurized the vessel, we captured the spent nitrous oxide and ethanol vapors in a balloon and passed it around to test for effect.

The combination of ethanol vapors and laughing gas was ragged in all our (4 people) lungs, so there are clearly limits to how much you can breath.
 
KLITE

KLITE

Well-Known Member
@Fadedawg

Had an attempt at it with whatman filter, mixed ethanol when butane was nearly gone in the splatter platter and froze it for 2 days before filtering.

Put it on pyrex posterior to filtering 45C to evaporate, when at aviscous consistency poured off onto parchment got it as thin as i could and into oven at 45C to vacuum.
16h later no more bubbles present, had a huge dab tasted right a lot terpier than i imagined itd turn out, put lighter to a few samples take from dif parts of the slab and theres no weird fire or sparks. However it is not shatter :( its tough but not brittle slightly tacky. Material is abt month old and its been frozen the moment it was bone dry. Any advice on method improvement to get it to that desirable consistency?
 
KLITE

KLITE

Well-Known Member
@Fadedawg

Man last night i decided to not be afraid and try purging the way you/youse have said. Put that shit at 115F (when im scared to ever let it go over 35C) and what a fucking result bro! I purged to completion an 8 g puddle in about 10 hours!!!!! It would have taken me 4 or 5 day witt my previous method and im quite sure it would not take all butane out. It came out aromatic as fuck and a trim run is shattering at room temp! With my previous method same strain would always turn out a bit sappy.

To be honest the couple of times i had the chance to speak to a qualified chemist and told them i would vacuum something for days they kinda chuckled and said that degassing under a vacuum should be a ''fairly'' quick process, definetly shouldnt take longer than 24 hours was the impresson i was under.

Anyhow a little festive pic for you.

IMG_20170106_043142.jpg

Next batch ill try making absolute again with the advice you been giving. With the thin film technique how long does it take you to fully purge a good size slab with your parametes?
Ive met my friend again and hes explained his absolute process again. He says after filtration he puts just enough ethanol on the pyrex to make a puddle that wont! reach any of the corners, 10 12 min at 60C you scrape at most 0.2 of what appears to be a bar of crystals.
 
Fadedawg

Fadedawg

Well-Known Member
KLITE said:
@Fadedawg

Had an attempt at it with whatman filter, mixed ethanol when butane was nearly gone in the splatter platter and froze it for 2 days before filtering.

Put it on pyrex posterior to filtering 45C to evaporate, when at aviscous consistency poured off onto parchment got it as thin as i could and into oven at 45C to vacuum.
16h later no more bubbles present, had a huge dab tasted right a lot terpier than i imagined itd turn out, put lighter to a few samples take from dif parts of the slab and theres no weird fire or sparks. However it is not shatter :( its tough but not brittle slightly tacky. Material is abt month old and its been frozen the moment it was bone dry. Any advice on method improvement to get it to that desirable consistency?
Click to expand...
High monoterpene content will leave it a pull and snap soft, but you should be able to roll it between you fingers briefly without it sticking.
 
Fadedawg

Fadedawg

Well-Known Member
KLITE said:
@Fadedawg

Man last night i decided to not be afraid and try purging the way you/youse have said. Put that shit at 115F (when im scared to ever let it go over 35C) and what a fucking result bro! I purged to completion an 8 g puddle in about 10 hours!!!!! It would have taken me 4 or 5 day witt my previous method and im quite sure it would not take all butane out. It came out aromatic as fuck and a trim run is shattering at room temp! With my previous method same strain would always turn out a bit sappy.

To be honest the couple of times i had the chance to speak to a qualified chemist and told them i would vacuum something for days they kinda chuckled and said that degassing under a vacuum should be a ''fairly'' quick process, definetly shouldnt take longer than 24 hours was the impresson i was under.

Anyhow a little festive pic for you.

View attachment 3869634

Next batch ill try making absolute again with the advice you been giving. With the thin film technique how long does it take you to fully purge a good size slab with your parametes?
Ive met my friend again and hes explained his absolute process again. He says after filtration he puts just enough ethanol on the pyrex to make a puddle that wont! reach any of the corners, 10 12 min at 60C you scrape at most 0.2 of what appears to be a bar of crystals.
Click to expand...
We've gotten below 10% of FDA standards in about four hours, starting with cotton candy.

QWET takes longer, because of boiling point and viscosity differences, but never more than 12 about hours.
 
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