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co2 oil

vapeking

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Thanks i guess we'll try it out. How much bubbling should occur when doing a final vacuum purge to get remaining ethanol out of winterized Co2 oil? Barely see any bubbles and when U do its real slow like lava looking.
 

Gray Wolf

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Thanks i guess we'll try it out. How much bubbling should occur when doing a final vacuum purge to get remaining ethanol out of winterized Co2 oil? Barely see any bubbles and when U do its real slow like lava looking.

Lava like blurps, rather than fine bubbles, suggest retained alcohol.
 

vapeking

Member
Lava like blurps, rather than fine bubbles, suggest retained alcohol.

Can you explain what kind of bubbles we should see and why? Retained alcohol like if its still doing then the alcohol is still in the oil? There are fine bubbles as well, just not any violent bubbling going on.
 

Gray Wolf

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There are several things coming out of the puddle, that we've identified with a mass spectrometer residual gas analyzer. Water, solvent, terpenes, and CO2.

Water and solvent bubbles will tend to be random sized and larger, while in the back ground there will be small fizzy, more or less equally sized bubbles, produced by the exiting CO2 and the monoterpenes.

The small fizzy bubbles will sometimes combine and produce larger bubbles, but they are slower to inflate than solvent or water bubbles.
 

SkyHighLer

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GW, I want CO2 bubbles too! ;-) I never get small bubbles at the end, just sloooooooooowly forming big bubbles, I'm going to be running some Thin Mint Cookies with Lotus canned butane for sharing at the Cannabis Cup this weekend and know I'm not going to be seeing any "small fizzy bubbles," my procedure is 115F at down to -29.5" Hg for about forty-five minutes to an hour, I pull and release at the beginning until I'm no longer pulling a muffin. I've only been purging several grams at a time, but this always works for me, and my oil never waxes up.

Maybe the ongoing bubbling you're seeing is moisture??
 

Permacultuure

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Have you done any RST on any of your products? You only purge for 45-60 minutes is how I'm understanding it. That would explain why you won't see any small bubbles, I'd imagine there is quite a a bit of solvent in your extract still.
 

SkyHighLer

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Never tested my BHO, I've let the slooooooowly forming bubbles go on for a couple of hours, still no "small fizzy bubbles," and the big bubbles are at a fairly steady rate of bubbling after the forty-five minutes to an hour. I proffered my Lotus BHO, purged as described at Chalice, and was asked for repeat dabs, I couldn't tell the difference in behavior on the enails or in taste to any of the excellent oils offered to me in return. If a test of BHO purged to the simple standard I purge mine showed between 5,000 to 7,500ppm of butane I'd suggest the limit should be raised to 7,500ppm. Just saying my piece, so you know it, not willing to argue it at this time.
 

SkyHighLer

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Here, I'll even let you see my cookies. ;-))

The only "small fizzy bubbles" I saw were after boil off, pre vac, here's a picture of them, I'm sure you're all familiar...

Also a picture of the oil quiescent after forty-five minutes at 115F and vacuumed down to about the 20,000 micron level (-29.14" Hg.)

Picture of the oil at the end, the one hour point, notice no "small fizzy bubbles."

And a picture of the 'splat.'

Tastes nice to me, I'll have it with me at the Cannabis Cup this weekend to share, everyone loves girl scout cookies.
 

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vapeking

Member
we extract with Co2, then winterize, then rotovap then, then purge for 24 hrs. I believe at 29.5 at around 115 F. Do you think that is adequate to get residual alcohol out? We test every batch, but just for THC, CBD, CBN haven't tested for solvents, but it daps and doesn't pop and gets you where you need to be quick!! All our oil tests out between 45-65% THC and our CBD runs are about 30-50% CBD.
 

pluckfoo

New member
we extract with Co2, then winterize, then rotovap then, then purge for 24 hrs. I believe at 29.5 at around 115 F. Do you think that is adequate to get residual alcohol out? We test every batch, but just for THC, CBD, CBN haven't tested for solvents, but it daps and doesn't pop and gets you where you need to be quick!! All our oil tests out between 45-65% THC and our CBD runs are about 30-50% CBD.

when using the rotovap are you guys able to get all of the concentrate out or do you leave enough solvent for it to go into the next stage of purging?
 

Rotel

Member
Think of the rotovap as like a pyrex hot water bath in motion with a vacuum assist. Yes residual goods are to be reclaimed from the vessel with a solvent cleaning process. Call it the bakers dozen or my term, the devils cut. Lol makes for great mixed batch lab sharings.
 

vapeking

Member
comes out fairly easy, and what doesn't swish around with solvent and put into a waste container and re-winterize. All that waste adds up!!
 

Gray Wolf

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Never tested my BHO, I've let the slooooooowly forming bubbles go on for a couple of hours, still no "small fizzy bubbles," and the big bubbles are at a fairly steady rate of bubbling after the forty-five minutes to an hour. I proffered my Lotus BHO, purged as described at Chalice, and was asked for repeat dabs, I couldn't tell the difference in behavior on the enails or in taste to any of the excellent oils offered to me in return. If a test of BHO purged to the simple standard I purge mine showed between 5,000 to 7,500ppm of butane I'd suggest the limit should be raised to 7,500ppm. Just saying my piece, so you know it, not willing to argue it at this time.

Decarboxylation at 115F is painfully slow, so one way to learn to see the difference in bubbles, is to crank up the temperature and watch what happens at higher temperatures, once the solvent is gone.

The solvent isn't gone as long as there are, " big bubbles are at a fairly steady rate of bubbling".

If the butane hasn't been pre-distilled and there is significant pentane present, it takes more than a few hours to boil off. Better to take out before extraction.

My guess is they will be more likely to lower, rather than increase the residual solvent standards. Some are already calling for 50 ppm, or 100 times lower.

FDA standards for Class 3 solvents is as follows:

Solvents in Class 3 (Table 3) may be regarded as less toxic and of lower risk to human health. Class 3 includes no solvent known as a human health hazard at levels normally accepted in pharmaceuticals. However, there are no long-term toxicity or carcinogenicity studies for many of the solvents in Class 3. Available data indicate that they are less toxic in acute or short-term studies and negative in genotoxicity studies. It is considered that amounts of these residual solvents of 50 mg per day or less (corresponding to 5,000 ppm or 0.5 percent under Option 1) would be acceptable without justification. Higher amounts may also be acceptable provided they are realistic in relation to manufacturing capability and good manufacturing practice (GMP).

The other question of course, is what is n-Butane's human sensory threshold, and it is actually pretty low at 2.8mg/M3 (~2.8 ppm), so we should be able to smell/taste it far below levels of concern.

http://www.timestream.com/vgh/downloads/NO2articles/Ruth%201986.pdf

How long it takes to purge to those levels, depends heavily on what you are purging and its previous processing.

Some raw extracts are more viscous than others, so some require more heat than others to lower the surface tension enough for the bubbles to escape under vacuum.

The other thing is of course previous processing. The amount of time it takes to purge open blasted oil, or oil passively extracted, is greater than for instance, Terpenator cotton candy shatter using pre-distilled butane and finished under high vacuum, which already has more of the solvent gone.
 

Gray Wolf

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we extract with Co2, then winterize, then rotovap then, then purge for 24 hrs. I believe at 29.5 at around 115 F. Do you think that is adequate to get residual alcohol out? We test every batch, but just for THC, CBD, CBN haven't tested for solvents, but it daps and doesn't pop and gets you where you need to be quick!! All our oil tests out between 45-65% THC and our CBD runs are about 30-50% CBD.

Ethanol is harder to get out than butane or CO2, so takes longer.

How purged would depend on how thin the film. That is long enough for a thin film.

Ethanol is easy to taste and the human sensory threshold for it is about .34 mg/M3(~.34ppm).

http://www.timestream.com/vgh/downloads/NO2articles/Ruth 1986.pdf

Seeing it on a GC is hampered by the ethanol spike falling right under the alcohol injection spike.
 
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