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purging without vacuume?

Gray Wolf

A Posse ad Esse. From Possibility to realization.
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From 115F to 125F? Backing the vacuum back down to accommodate the increased heat or staying at -29.5"Hg? I haven't tried purging that hot yet in an effort to avoid degradation and terpene loss but I'm going to be collecting terpenes via other methods anyway I think.

I'm really digging into Ernesto Reverchons work on SCFE Terpene extraction as an alternative to steam distillation but without multiple separators I don't see myself getting very far. Perhaps collecting via cold trap and vacuum oven immediately after extraction but before filtration would be better.

125F @ -29.5" Hg.

Bright guy, but not familiar with Ernesto's work on terpene extraction; reference?

The terpenes that I extracted passive SCFE tasted like alfalfa, but Paddy shared some that had been fractionated on the way down using multiple separators, and it exhibited both exceptionally good aroma and flavor.

Last I heard he was consulting as a free agent if you are interested in picking his keen alleged fine minds. [FONT=&quot][email protected][/FONT]
 

SkyHighLer

Got me a stone bad Mana
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As smooth as you always claim your dabs to be ;) I would like to suggest that non-distilled cans of "butane" leave a mystery oil that isn't too pleasant on the throat and lungs all the time, and some are more sensitive to it than others. While you are correct about the boiling points under vacuum (even as far back as your original posts on the subject), I think a deeper vacuum and/or a longer purge effectively removes this odor and harshness. Everyone I give dabs to on a daily basis (myself and labmates included) can attest to my dabs being smoother with longer purge times when I know my gas is "dirty". When I am properly operating my loop and distilling 50lb tanks almost daily, I can't say this trend exists at all. I have often smoked the dusty shatter left by my collection pot without any vacuum purge, beyond the final 15 minutes of solvent recovery. I don't think small amounts of pure butane hurt my throat, nor does it taste funky.
Butane is much more volatile than some of that canned residue.

With distilled solvent, I don't drop under 10,000 microns either. 85-90°F generally.

Is it mystery oil (non-volatile residue) or minute amounts of pentane/iso-pentane etc. (the semi-volatile residue) that you're detecting? I'm well aware there's a wee bit of these semi-volatiles in canned butane, I see them slowly boil off in my mystery oil test bags, just after the butane completely flashes off, I reduce the heat at the end just to observe this, though it's not something I report on, it's maybe a single drop, not much, but that's why I make sure my oil is liquid under vacuum, i.e., 115-120F, so when I take it down to -29.5" Hg, and after pulling a couple of muffins, and the bubbling is slowed to eternal time, under an hour for me, I know I'm clear enough of residues that no one can sense them.

Just my two cents, I think you guys got it backward, way too much time and concern on purging (I realize there are regs, sorry, I believe they're based on bs,) all the while the push is on for high fractional distillation rates, a process which does benefit from TLC.

Sorry if I come off as rude/demanding, the undertone I hope you get is if you've been blessed with the mind to, question everything. For instance, come over to my house, and we'll compare dry hits off a calibrated temp controlled source one after another. :biggrin:
 
125F @ -29.5" Hg.

Bright guy, but not familiar with Ernesto's work on terpene extraction; reference?

The terpenes that I extracted passive SCFE tasted like alfalfa, but Paddy shared some that had been fractionated on the way down using multiple separators, and it exhibited both exceptionally good aroma and flavor.

Last I heard he was consulting as a free agent if you are interested in picking his keen alleged fine minds. [FONT=&quot][email protected][/FONT]

I'm a big fan of Patricks work and he is absolutely correct, fractioning in SCFE requires stepping down in pressure over multiple vessels to allow the targeted compound to crash out of solution. Waters achieves this via multiple separator vessels and automatic back pressure regulators. Eden has been ignoring it entirely and disavowing responsibility as they aren't cannabis processors and have an imperfect understanding of how SCFE works in regard to cannabis. I've been sharing a lot as they are building us a very large machine that is very expensive but there are engineering issues in the way still that will need to be overcome in another design.

I utilize their equipment and processing guidelines I developed largely in part due to your work with cannabis along with H Perotin-Brunel and Reverchon while adhering to some very basic rules that I observed were static regardless of solvent. I aim to try to retain terpene content but its still imperfect without more control over the separator conditions.

The forum gates me at 1MB PDF files and the one I have for you is 3, do you have an email I could send it to?
 
Just my two cents, I think you guys got it backward, way too much time and concern on purging (I realize there are regs, sorry, I believe they're based on bs,)

I think that this is a huge issue in our industry actually. Most of the purging techniques that people are following are pseudoscience and not based on actual data. A lot of people degrade their product purging too long, too hot, too much agitation or contamination during flipping stages leaving it for days or weeks "just to be certain" rather than establishing procedure based on observable data. They rush for shatter not knowing why it's even a desirable end product or IF it's a desirable end product. (I don't think it is personally, I think rough extractions are on their way out and polished, purified, isolated, compounded products are the future but that's just me)
 

Old Gold

Active member
SH:
You could be right about pentane. And I will say the sources are inconsistent, and I have noticed some residues slowly boil/evap away. Whip-It 5x surprisingly impressed me in that regard, left no trace of smell after a few hours (maybe as long as a day) at room temperature, no vacuum. But some of the non-volatile yellow stuff I could taste a week later, after sitting at 90-100°F. I haven't tried purging that mystery oil alone. I'd like to distill a large batch or three and see how it all reacts under vacuum, without the surface tension of cannabis oil holding it in.

I'm gonna take you up on that offer, I don't have a clean, accurate heat source at the moment, and I'm trying to give my lungs a break for a few weeks by eating some distillate as much as possible.

Thomas@LRL: But also, with proper care, those extra measures "just to be certain" can include a higher temperature and pressure closer to atnospgere, or could be lower temperatures at a deeper vacuum. And to say that you cannot purge for, say, 2-3 days without "degrading" the product is silly IMO. Sone people may degrade their product, but what a broad generalization. What do you define as degrading?

Purified/isolated compounds are of utmost interest to me as well, but the average home botanist mother of however many (for example) does not necessarily NEED to isolate any of her compounds, nor does she need to spend much time or money on extraction. Nor should she have to purchase some bourgeois"designer" dabs from a storefront. A standard, relatively clean butane extraction that leaves little or no solvent behind is good enough, should she feeling safe enough about her methods.
 
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Thomas@LRL: But also, with proper care, those extra measures "just to be certain" can include a higher temperature and pressure closer to atmosphere, or could be lower temperatures at a deeper vacuum. And to say that you cannot purge for, say, 2-3 days without "degrading" the product is silly IMO. Sone people may degrade their product, but what a broad generalization. What do you define as degrading?

From a procedural standpoint its possible to alter temperature and pressure variables, but the biggest issue is one of ignorance. They've been told they need these pieces of equipment and what they're used for but they aren't getting a deeper explanation than "It removes solvents". My experience is entirely anecdotal but I see a lot of people locally who are attempting to speed up processing by pulling a deeper vacuum and increasing the heat without knowing why, or trying to preserve terps and not nucleate (another poorly understood phenomenon) by going lower temperature albeit the same deep vacuum for as long as two weeks in some cases. In every case it was "someone told them that someone did it this way and got the best most dopest shatter/wax ever".

It's easy to remedy, I link them the charts that SH was kind enough to prepare a long time ago, and Grey Wolfs work on solvent removal, and any other literature source to explain what altering those details achieves, why one might want to, how to properly choose a vacuum source for your application, why you might put a cold trap between oven and pump etc *Without charging them for information that is readily available for free online
 

Gray Wolf

A Posse ad Esse. From Possibility to realization.
Mentor
ICMag Donor
Veteran
I'm a big fan of Patricks work and he is absolutely correct, fractioning in SCFE requires stepping down in pressure over multiple vessels to allow the targeted compound to crash out of solution. Waters achieves this via multiple separator vessels and automatic back pressure regulators. Eden has been ignoring it entirely and disavowing responsibility as they aren't cannabis processors and have an imperfect understanding of how SCFE works in regard to cannabis. I've been sharing a lot as they are building us a very large machine that is very expensive but there are engineering issues in the way still that will need to be overcome in another design.

I utilize their equipment and processing guidelines I developed largely in part due to your work with cannabis along with H Perotin-Brunel and Reverchon while adhering to some very basic rules that I observed were static regardless of solvent. I aim to try to retain terpene content but its still imperfect without more control over the separator conditions.

The forum gates me at 1MB PDF files and the one I have for you is 3, do you have an email I could send it to?

Thanks! Ah wayte with bait on mah breath!

[email protected] will accept up to around 15.
 
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