What's new
  • Please note members who been with us for more than 10 years have been upgraded to "Veteran" status and will receive exclusive benefits. If you wish to find out more about this or support IcMag and get same benefits, check this thread here.
  • Important notice: ICMag's T.O.U. has been updated. Please review it here. For your convenience, it is also available in the main forum menu, under 'Quick Links"!

Purging winterized BHO

JColtrane

Member
Is it possible to completely purge ethanol off at low heat ... like 100, and with the add of a strong vac (got an edwards rv12). I've made my resin sheet micro thin by flattening it, and streching while it's in a taffy state. I've had a hard vac for over 15 hrs and still flexible. Will it ever shatter, or do I need higher heat? The piece is about 8 or 9 grams ... maybe I should try to purge 2-3 gram increments. Any help? BTW still seeing small bubble, not many, but there's a few ... which leads me to believe there's still ethanol in it.:thank you:
 

Aeroguerilla

I’m God’s solider, devil’s apostle
Veteran
i get shatter everytime all i do is put the pyrex in the oven on the lowest setting... mine is 170 i believe. i just leave it till no more bubbles and when she cools its like breaking glass... you dont need a vac to get shatter
 

Hammerhead

Disabled Farmer
ICMag Donor
Veteran
I just made some... Yes you can. I put a pyrex dish with water heat that to 40c put the jar with the oil and wait.
 

JColtrane

Member
What if I did want to use the vac/chamber system ... would 125 be a good temp? Right now it's a thin film, and lightly bubbling at 125. Should I just wait till stops bubbling?
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
What if I did want to use the vac/chamber system ... would 125 be a good temp? Right now it's a thin film, and lightly bubbling at 125. Should I just wait till stops bubbling?

That would be hot enough, but we've never had to go above 115F at -29.9 Hg to get the bubbles to break.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Gray, not sure I have heard you mention how long you purge for though at that temp.

It varies depending on the material, but I do it in thin films until the irregular bubbles stop forming, which usually only takes an hour or two.

We typically produce shatter instead of wax, so long pumping isn't required.

The best butane test that I've found is taste, as we can taste it long after it is below levels of health, or singed eyebrow concerns.
 

JColtrane

Member
Okay GW ... could you explain the difference in bubbles please? Cuz I might have over purged. 120 @ -29.9 hg hard vac for about 12 hrs, and held pressure under mild heat for another 8 hrs. I get a flexible snap oil. Taste is so, so ... but strong. Might just use it for tincture ... Gonna keep playing around though, thanks for the inspiration :)
 

CannabisTHC

Member
The small uniform bubbles are said to be the decarboxylated bubbles. The solvent bubbles are the irregular larger sized bubbles. But at 120 degrees I'm not sure decarboxylation would be happening unless its been under heat for a very long time which it sounds like you are doing, I know there is a graph GW has somewhere explaining this.

JColtrane, how do you purge with heat under vacuum? Just curious since I'm trying to figure out how I'm going to do that. Whether that be a ceramic plate heated in the oven or a digital hot plate inside the dessicator or a vac oven.
 

Bluewidow

Member
The small uniform bubbles are said to be the decarboxylated bubbles. The butane bubbles are the irregular sized bubbles.

JColtrane, how do you purge with heat under vacuum? Just curious since I'm trying to figure out how I'm going to do that. Whether that be a ceramic plate heated in the oven or a digital hot plate inside the dessicator or a vac oven.

If your purging your oil at temps where decarboxylation is taking place are strickly far too high, you don't want you BHO decarb'd unless your eating it. As far as butane bubbles looking a certain way, again I can't agree with that statement either.
 

CannabisTHC

Member
If your purging your oil at temps where decarboxylation is taking place are strickly far too high, you don't want you BHO decarb'd unless your eating it. As far as butane bubbles looking a certain way, again I can't agree with that statement either.


Yes I'm well aware the oil is too hot if its decarboxylating for smoking, the idea is to keep the temps at 110-140 to keep as many terps as possible for the smelliest/tastiest product when purging butane. I'm answering JColtrane's question to tell when your done purging solvent bubbles and its well known that the irregular larger bubbles are said to be solvent bubbles and the decarboxylated co2 bubbles are the small uniform bubbles.

JColtrane, I've seen GW say that he won't use heat when evaporating ethanol when under vacuum, he'll reach at least -29.5hg.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
Okay GW ... could you explain the difference in bubbles please? Cuz I might have over purged. 120 @ -29.9 hg hard vac for about 12 hrs, and held pressure under mild heat for another 8 hrs. I get a flexible snap oil. Taste is so, so ... but strong. Might just use it for tincture ... Gonna keep playing around though, thanks for the inspiration :)

The solvent bubbles vary in size, with some quite large. Decarboxylation CO2 bubbles are smaller, of more uniform size and more fizzy.

Decarboxylation also occurs at 115F, though more slowly than at higher temperatures, as evidenced by the CO2 bubbles produced, although the graph that Jump posted doesn't clearly show it. The rate of conversion of THC to CBN is very close to the same rate as THCA is converted to THC, at that temperature.
 

Attachments

  • Decarboxylation graph-1-1.jpg
    Decarboxylation graph-1-1.jpg
    52 KB · Views: 16

Rowdy420

Member
Glad to see the 170 oven trick is catching on, I usually check the pyrex every 10 minutes to see the progression in bubbles. In past runs in the oven I have taken it till there was no bubbles but, as stated above it removes terpenes the longer you heat. The last run I pulled a little early when the smallest bubbles start to break and let sit out in a cupboard for at least a week. Once "aged" it is some of the tastiest I've run, so for GW to recommend lower and slower I'm all over it. Just going to have to up-grade to some better equipment other than on oven!

Good luck, Peace
 

Lebniis

Member
Came across a method that might help some purge off ethanol or everclear using a vacuum chamber and heat source.

Once you have purged for a while and there seems to be a lull in bubbles popping, stop the vacuum, open the chamber and spread the oil as thing as possible. Usually the bubbles pop and form small areas of no oil on parchment paper. Using another piece of parchment spread it from center out or whatever method to get it even. Stick the piece you used to spread onto the oil and freeze to make it easy to not lose any oil. So far this is working to release many bubbles with 'rainbow' tint and random size.

This might help with those trying to keep temps below 120. Otherwise it is difficult to keep the oil thin enough.
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
We purge ethanol in thin films under vacuum, using a hotplate inside the vacuum chamber, using a 6" Petri dish and 115F. As long as the film is kept thin enough, all that is necessary is to keep track of bubble production, so that we know when to stop.

In super thin films, decarboxylation also happens faster, so it is important to remove it from the hot plate when the large irregular bubbles stop and only the small fizzy bubbles remain, so as to retain it in carboxylic acid state.

It typically takes about one to two hours to fully purge and when the starting material is young, produces a flint hard brittle resin chock full of good flavors and odors.

We are a small research lab, and use small equipment, so sizing for larger volume might include something that does the thin film evaporation faster, such as a rotary evaporator.

We are building a prototype rotary evaporator this year that is oriented more toward cannabis resin harvesting and is easier to clean than a conventional Rotovap, but it will operate on the same principles, so you might check out http://en.wikipedia.org/wiki/Rotary_evaporator for process details.
 

FouRtwizzle

Member
I recently tried to winterize 5 grams of wax i picked up at a local shop.

After freezing the solution for 24 hours, I removed 1.9 grams of plant waxes and other matter. I was left with 3.1 grams of final product.
I got the temps too high and lost a lot of terps but its real potent.
I'm looking forward to improving my tech and making a true absolute that will test in the90's ofTHC content!


Here are some pics.

The images with the coffee filter and the parchment paper are the plant waxes which I removed.

image-1.jpg


image-3.jpg


image-5.jpg


image-6.jpg


image-7.jpg
 

Latest posts

Latest posts

Top