Steam distillation of winterized absolute

[Chonkski]

I just got a fractional distillation setup and have been messing around with distilling water and dlimonene and in a few days will be giving some low quality oil a try. The boiling points under vacuum im still trying to figure out so ill probably just wing it and collect a few fractions and send them in for testing to see what i got. Was going to use dlimonene as my carrier? I dont know if thats correct though, was just a thought. Would i be able to collect the THC or CBD fractions im looking for and leave the dlimonene behind with any other undesirables since it has a higher BP then THC?

Heheh! This is exactly my plan as well!!!!!!!!!!!

To the T. I have a ton of d Limonene and a ton of winterized high grade bho.

Literally just posted the same thing in another thread.

Glad someone else is on for experimenting!

 

[Chonkski]

What setup you using? got a pic?

I'm curious as well, I'm still shopping.

If not a pic, perhaps a link?

 

[flatslabs]

Is the compound you are after already the one with the highest boiling point? If so, why use a buffer or re-condense that compound at all. From what I can see the BP of d-limonene is 177C and there are other Terpenoids or compounds which have higher BP, THC-V is ~220C for example.

http://cannabis-med.org/data/pdf/2001-03-04-7.pdf

 

[Chonkski]

Is the compound you are after already the one with the highest boiling point? If so, why use a buffer or re-condense that compound at all. From what I can see the BP of d-limonene is 177C and there are other Terpenoids or compounds which have higher BP, THC-V is ~220C for example.

http://cannabis-med.org/data/pdf/2001-03-04-7.pdf

Dlimonene happens to be the only easily attainable food grade terpene I can find, any chance you know of a good resource.

Perhaps I'll do some searching for Quercetin or Pulegone..?

Thank you for this, I added it to my reading list to for tonight

 

[G.O. Joe]

This is probably a noob question, but why steam distill the oil instead of just going from the start and steam distilling the plant matter? I assume there's a reason I never see anyone mention doing that

Anyone using conventional steam is doing it to remove butane impurities from BHO with the steam. Oil of Cannabis is almost all terpenes - if THC could reach its boiling point at atmospheric pressure, it would be over 400C/750F. Decent partial pressure still requires a higher temperature, compared to other things, so it would require a more extreme steam.

I have to imagine pharma and their subsidy counterpart chemical companies will figure it out as they did with opiates and amphetamines.

Synthetic opiates often come from opium, like fooling with codeine. Amphetamines are dead simple and cheap. THC syntheses need precursor olivetol - very expensive and not easy, even the best synthetic pathway starting from acetone and hexanal. The easiest and cheapest way to make olivetol is from CBD.

 

[G.O. Joe]

Yes vaporizing from plant material doesn't work as well as THCA, which doesn't work as well as THC. This is what happens in a Volcano, from Hazekamp's thesis.



If I was going to try something on-topic, I'd modify a microwave oven. After destroying the first three, the fourth experiment would fail spectacularly and I'd give up. You might be able to make your own SFME though. That doesn't mean it would distill THC, but you could still show it off.

 

[grow nerd]

Also, I don't think this application requires fractioning. Remember, we want the distillation path to be as short as possible and all we are trying to do is separate the cannabinoids so you don't want to add a big column and you aren't trying separate a bunch of different things, all you want to do is keep the good stuff and distill off the bad stuff.

I suppose you could collect off some terpenes first, but I would leave that for a further experiment once you get your refinement process down.
And that last link you posted is 22/40 joint size, for this application you want 19/22 to minimize loss. The only distillation setup I have access to is 1L to 500ml and has 24/40 joints, so I would need a lot of starting material to use that apparatus.

I'm having a hard time trying to understand why the bad stuff has to be distilled first to be removed, rather than just being boiled off with no distillation or collection, if all you're trying to do is leave behind the good stuff with the bad stuff supposedly having lower boiling points.

I assumed the process had more to do with condensing (good) vapor from a BHO sample, possibly after boiling/vaporizing off the bad stuff, including whatever impurities that makes old oil dark and taste bad.

The way I understandand and interpret your process, you are simply trying to vacuum purge at a high(er) temperature with a bunch of fancy glassware unnecessarily connected in between.

What happens to BHO when "cooked" in the microwave? Does it turn into liquid/vapor?

 

[grow nerd]

I stuck a piece of shatter into the microwave for up to 1 minute on a glass dish, but didn't seem to have any vaporizing or heating effects. It did eventually heat the tiny sample indirectly through heating the dish.

 

[Pure777Extracts]

http://skunkpharmresearch.com/vacuum-equipment-and-process-tips/ glad to see things moving in a positive direction this should help with your vacuum boiling points

 

[grow nerd]

Any new info to add that almost everyone isn't already aware of?

 

[Pure777Extracts]

what did you think I was showing you?

 

[grow nerd]

The way I'm perceiving it is that you keep acting like you already know the process, yet have added nothing but "chime in" with info that most people in the discussion were long aware of, and has already been discussed and generally accepted to be understood. Along with status updates on how busy you are on big projects.

If you have the answers and are so eager to share, why don't you, already? Rather than follow along every discussion and echo/regurgitate info only after it's already been widely discussed and act like it's breaking news?

I apologize if I've misread your intentions after noticing what I felt was a pattern in your posts, but it's quite confusing what you think you are adding besides showing and confirming to everyone that you are also now informed on certain data sets? (Which I find mildly annoying on its own.)

 

[Pure777Extracts]

sorry but from what you guys were discussing I thought you needed it...

 

[MEMED]

adept def has the process down. Ive sent you a couple emails adept. Im curious if your getting them, perhaps there going to spam? Should I DM?

 

[Pure777Extracts]

No I haven't

 

[grow nerd]

If you don't know, but are seeking to find out like everyone else, just say so and join in the efforts rather than trying to play the noble, all-knowing one. There is no shame in not knowing everything. It would be more productive for everyone.

adept def has the process down.

How did you come to this conclusion? Just the fact that this "extract company" who claims all the knowledge on "solventless" / "clear", yet does not have a product available? And has, to date and to my knowledge, only repeated info posted by others that has already been long discussed?

Kinda like you were on TickleMyBalls' ... erm, balls, before it was publically demonstrated that he knew close to nothing useful while acting like he had all the privileged secrets?

My guess is that adeptextracts' solventless product release date will coincide with the public discovery/release date of the technique.

Maybe I just need Hey-soos.

 

[grow nerd]

I hate the Internet. Makes me unhappy unnecessarily.

Would be interesting to live in an era where selling drugs isn't/wasn't so complicated.

 

[G.O. Joe]

I stuck a piece of shatter into the microwave for up to 1 minute on a glass dish, but didn't seem to have any vaporizing or heating effects.

That's why I suggested adding saltwater to oil in the other thread, and mentioned that pot has been dried in the microwave for over 30 years, but I have yet to hear of the oven zapping potency.

Liquid polar molecules and ions do the heating in microwaves.

 

[Gray Wolf]

If you don't know, but are seeking to find out like everyone else, just say so and join in the efforts rather than trying to play the noble, all-knowing one. There is no shame in not knowing everything. It would be more productive for everyone.

Maybe I just need Hey-soos.

If I have learned anything from this and other forums, it is that there are no noble all knowing ones walking amongst us mortals, but there is a community of folks sharing what snippets of the puzzle that they do know, which we put together as a group until eventually one of us has a brain fart and drops in the last piece.

Formal brainstorming techniques used in corporate think tanks, suggests that it is a mistake to apply judgement to input, until it has run its course, because small insignificant, even risible inputs, often are the seed that someone else elevates to the next level.

One of the complaints that I receive from some of the most brilliant people I know, is that they don't participate or share on the forums, because some folks can't stay focused on the central thread and divert the conversation to focusing on perceived personal flaws in the messenger.

I wish they were on line sharing, because it is our communities loss, so I suggest that it is counter productive to do more than ignore input that you feel is irrelevant, because it isn't necessarily irrelevant to everyone and publicly denigrating the messenger discourages them from sharing the useful insights that they do have.

On the subject of steam distillation, I have no direct input or experience, other than having tried clear extracts by the mystery process while consulting at an oil producer who had some low grade oil processed by them to see how it came out.

I note it was totally devoid of any mono or sesquiterpenes at the level of sensory perception. It is more pasty than resiny, and has a clouded light amber appearance, such as a colloidal suspension of things like wax might produce.

It was smooth vaporized, with a pleasant, albeit bland taste, and had a slow arriving, but long lasting high. Perhaps if it were made from prime oil, the high would have arrived faster and higher, but I have no personal experience to support that tongue in cheek observation.

There was absolutely zero sensory perception of any solvent residuals.

Perhaps we will know more after my client further processes it in a vacuum oven, to see what products are possible, and decides what parts to share.

 

[flatslabs]

I'm having a hard time trying to understand why the bad stuff has to be distilled first to be removed, rather than just being boiled off with no distillation or collection, if all you're trying to do is leave behind the good stuff with the bad stuff supposedly having lower boiling points. I assumed the process had more to do with condensing (good) vapor from a BHO sample, possibly after boiling/vaporizing off the bad stuff, including whatever impurities that makes old oil dark and taste bad.

I was speaking in an ideal world in which you would leave behind the good stuff, and it is not a distillate itself. This was more to address federal law about processing controlled substances than anything, read a few of the posts that GO Joe made. I wasn't trying suggesting the actual working process leaves behind the goodies.

The way I understandand and interpret your process, you are simply trying to vacuum purge at a high(er) temperature with a bunch of fancy glassware unnecessarily connected in between.

Vacuum AND Steam both lower the boiling points of organic compounds. If I was setting up a 4 -5 hour long steam distillation under hard vacuum, I am probably going to want a separatory funnel dripping water into my boiling flask the whole time so it doesn't dry out, not something easily accomplished in a vacuum oven, not to mention the precise temperature control and even heating. All that "unnecessary" glassware is exactly what you need to do that.