Absolute separated from Concrete?

[cannabinoid]

Ok so last night and tonight l decided to turn my concrete into an absolute, if l can call it concrete, it's in shatter form at room temp, but l ran it from dry trim instead of fresh, so is it an oleresin or however its said?? Anyways!! Back to the BHO BHC chunk that im dissolving into this beautiful everclear

The everclear BHO mixture became very cloudy with white, waxy particles just liked you guys showed said. Then l froze it for 24 hours just for a lil extra. Well it started to suspend like a cloud and some sank a little, note this was very good, clean tasting BHO in shatter form at room temp. So l guess there are some waxes or something else left in there...

So l take the glass out tonight, 24 hours later and filter it through a brown coffe filter l had at the house. Unbelievable the wax or whatever it ended up filtering out.

So l just warm water bathed it really low and slow like l do my oil without the flame purge of course haha and scraped it up

lt is still shatter, maybe a LITTLE harder not much at all. But it is a little darker in color, still golden still beautiful. lt hits smoother like this in the absolute form or whatever, but it does take away that lemon zest it had before and l really do enjoy that taste and flavor. l guess that is what the waxy shit is l don't know, have no idea. Still debating if it's worth the extra work...

i think the terpene that gives the lemon flavor is rather delicate and extra care w/ low temps needs to be utilized. my guess is the second exposure to the warm water bath (which normally you don't do) just further degraded some of the lemony terpenes. not to say the final product is not purer, just may not have all the appealing terpenes the original flower had.

 

[jump]

it does take away that lemon zest it had before

the absolute is free from all the bubbles and looks like glass

From the observation that the lemon zest was gone along with the bubbles,
you can make a formal logical conclusion that bubbles are the bearers of lemon zest. :) I’m kidding!

i think the terpene that gives the lemon flavor is rather delicate and extra care w/ low temps needs to be utilized.

Perhaps also w/ low oxygen.

 

[spinkus]

So the next time l make an absolute from my BHO how should l evaporate the alcohol out? Should l just let it sit out at room temp until it evaporates off instead of the hot water bath method? l did it really low and slow like l do when l make the BHO for that very reason, not to boil off any flavors

How long will it take for it to evaporate 200ml of everclear at room temp?

 

[jump]

Theoretically recommend a vacuum distillation,

but I have no vacuum and I distill ethanol in portions of 50 ml on a steam bath,

which provides about 160F on the surface of the evaporator plate.

Obvious that such heating is not useful for keeping terpenes.

In the experiments of evaporation at ambient temperature,

I noticed faint shades of vodka in taste.

 

[spinkus]

Thanks for the reply and info jump. Yeah l definitely dont want added hints of vodka flavor in my absolute, kind of defeats the purpose l would think.

l guess l will do it over a low steam bath like last time. Since thats about all l can do. The absolute does taste so much smoother, even without the lemon terpenes im still thinking it tastes better. lm just gonna have to do another run and experiment a little

 

[cannabinoid]

^ jump is the man when it comes to EtOH

 

[TheBigDabowski]

Theoretically recommend a vacuum distillation,

but I have no vacuum and I distill ethanol in portions of 50 ml on a steam bath,

which provides about 160F on the surface of the evaporator plate.

Obvious that such heating is not useful for keeping terpenes.

In the experiments of evaporation at ambient temperature,

I noticed faint shades of vodka in taste.

I do have access to a VAC that we use to make BHO. I did do a run this weekend that I would like to try to make into absolute using this process to create a more pure product. I had some questions for you or anyone who is knowledgeable and has done this.

Here is what I am working with right off of the VAC. It now turned into a shatter with lots of darkness to it which is why I want to attempt to create an absolute.

http://i9.invalid.com/albums/a77/TwizteD25/IMAG0238.jpg

1. It seems like I just mix the ethanol with the BHO.
2. Set it into the freezer for about 24 hours.
3. Use coffee filter to separate the absolute from the concrete.
4. Purge using heat as suggested or VAC.
5. Enjoy that absolute amber!

How much ethanol should I use, jsut enough to cover the BHO or a good amount above it?

Also you mentioned you would rather VAC than use heat. If I were to VAC instead, would a melt vac once be enough or would it need to be done a few rounds such as with butane purging.

Last question, how will I know all of the ethanol has been purged?

 

[jump]

Ethanol is needed in such quantity that the solution has turned out quite liquid for further filtration after cooling.

The excess ethanol will only lead to its loss,
the lack of ethanol will make the solution too viscous,
making it difficult to filter and leave resinous trail on the filter,
which after drying the filter can be cut with scissors and washed well with ethanol.
In my small practice, consumption of ethanol is about 50 ml / 0.7-1.0 g of resin.

For the use of a vacuum, I can only theorize.
On the practical experience of application of vacuum to ethanol reported GrayWolf.

Using the vacuum does not remove the need to melt the resin for the mobility of the solvent at its disposal.

 

[Graywolf]

Ethanol is needed in such quantity that the solution has turned out quite liquid for further filtration after cooling.

The excess ethanol will only lead to its loss,
the lack of ethanol will make the solution too viscous,
making it difficult to filter and leave resinous trail on the filter,
which after drying the filter can be cut with scissors and washed well with ethanol.
In my small practice, consumption of ethanol is about 50 ml / 0.7-1.0 g of resin.

For the use of a vacuum, I can only theorize.
On the practical experience of application of vacuum to ethanol reported GrayWolf.

Using the vacuum does not remove the need to melt the resin for the mobility of the solvent at its disposal.

Yeah, what Jump said!

 

[squiggly]

Yeah, what Jump said!

From wiki:

Coprecipitation is an important issue in chemical analysis, where it is often undesirable, but in some cases it can be exploited. In gravimetric analysis, which consists on precipitating the analyte and measuring its mass to determine its concentration or purity, coprecipitation is a problem because undesired impurities often coprecipitate with the analyte, resulting in excess mass. This problem can often be mitigated by "digestion" (waiting for the precipitate to equilibrate and form larger, purer particles) or by redissolving the sample and precipitating it again.

/wiki

In this case we can think of the oil as coprecipitating the solvent particles which would normally be dissolved in the air under vacuum. These impurities are of the occlusion type where the coprecipitated molecules become physically trapped within the lattice of the precipitate. In this case, instead of being stuck in a crystal lattice, the molecules are trapped within the hyrdrogen-bond/hydrophobic interaction networks of the surrounding oils.

 

[TheBigDabowski]

So VAC purging may not work or did I read that wrong? Also I had a tough time getting the butane out of that last batch (never got it out to my liking) and was wondering if the ethanol will be as difficult or will it not get trapped such as the butane making it hard to purge. Also what if some leftover ethanol were to be left in the oil and to be vaporized would this be a concern?

 

[squiggly]

So VAC purging may not work or did I read that wrong? Also I had a tough time getting the butane out of that last batch (never got it out to my liking) and was wondering if the ethanol will be as difficult or will it not get trapped such as the butane making it hard to purge. Also what if some leftover ethanol were to be left in the oil and to be vaporized would this be a concern?

The lower the boiling point the easier something will be to get out (this ignores polarity/complexation issues).

Vac purging will work--but only when the viscosity of the oil is low enough to permit release of the solvent. This is why you must heat the oil prior to/during vac purging.

 

[TheBigDabowski]

May give this a ty in a week or two. Thanks

 

[bobismyfather]

I vacuum purge directly after the Tamisium clean out with ethanol. It then goes down in temperature to about 6 degrees C during the vac.
I used to try and follow the warming procedure, but it goes against the idea of not heating. Also the notion of thin film is over rated. The solution level is no longer a concern for me.
After careful monitoring several purges of about 1 cm alcohol to dry resin, I now purge with no heat till dry. Takes a few hours and it's nice and hands off. The last 30 minutes I am present though to fine-tune the final product. (Dab up the little bit of water that appears after all the alcohol is gone, flatten out the extract for more even purge, not over pull, not under pull, etc.)

 

[squiggly]

Also the notion of thin film is over rated.

It most certainly is not--it's just difficult to pull off is all.

Believe me, if you had a rotovap (a thin-film evaporator) you would not be purging oils using anything else.

 

[bobismyfather]

Well, you just went from a few hundred bucks to a few thousand. And How does the resin exactly get removed from the chamber? Looks like the are a closed bulb.

 

[squiggly]

Well, you just went from a few hundred bucks to a few thousand. And How does the resin exactly get removed from the chamber? Looks like the are a closed bulb.

In my lab we do it in the containers they will stay in (little glass cylinders)--just put an adapter on the apparatus.

My point wasn't cost effectiveness. It was to say that thin film evaporation isn't overrated. It isn't. It's still far and away the most effective and efficient method for removing solvents (hence why it is the laboratory standard).

 

[rusty]

For the use of a vacuum, I can only theorize.
On the practical experience of application of vacuum to ethanol reported GrayWolf.

I made some absolute out of some mouldy buds a few weeks ago, I used the .2 micron syringe filter method, turned out great. One thing about using a vacuum to boil ethanol though, I used a single stage pump for the job, word or warning, the ethanol vapors mixed with the oil and messed up the vacuum on the pump. I think the pump is fixable, but the moral of the story is to use some sort of moisture condenser filter system inline with your pump and vac chamber, something like this (from tokecity):
http://www.kgw-isotherm.com/images/kf/s29.jpg
or here is greywolfs:

 

[rusty]

hmm, the skunk pharm link isnt working, u can find the image on this page:
http://skunkpharmresearch.com/getting-the-green-and-waxes-out-afterwards/
above the image of the syringe

 

[Mustard]

Is there anything one can add to their ethanol/bho solution to speed up the precipitation of the undesirables? Does activated carbon do this? What about a couple chunks of dry ice to instantly freeze it? Ill probably try the dry ice idea soon has anybody tried this?