What's new
  • Happy Birthday ICMag! Been 20 years since Gypsy Nirvana created the forum! We are celebrating with a 4/20 Giveaway and by launching a new Patreon tier called "420club". You can read more 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"!

Steam distillation of winterized absolute

Chonkski

Member
Also: I think it might be wise for those of us who wish to explore steam distillation to start a new thread


And so here we are!


Anyways, for those of you wondering. I am very curious to start experimenting with refining polished extract even further. Being able to put the title of 'solvent free' and achieving percentages of the 80's and up total cannabinoid, out of what was once poopy outdoor black goo bho.

I know this is becoming very popular, mostly on the consumer side. Which makes finding out specifics of the process a bit harder to find, many are trying to hide/cover up processes as well.

So this may be the forum where all of that can come to light! Then we can go ahead and rush towards the next big thing, lol.

I am no bio chemist major, so any help on the process would be greatly appreciated. I just have a lot of time and material to experiment with so I will document how my experiments go here.

Hope others share the same interest as I!
CK
 

Chonkski

Member
After doing some window shopping, I'm very interested in the setup DabGenius has.

Would it be probable to use this fancy rotovape with a reactor to refine winterized absolute even further?
 

Attachments

  • image.jpg
    image.jpg
    57.4 KB · Views: 14

Chonkski

Member
I think to start getting my feet wet, I will do some experimentation with a short path vacuum distillation apparatus. I will start by trying to fractionally distill winterized bho.
 

Attachments

  • image.jpg
    image.jpg
    34.8 KB · Views: 14

Chonkski

Member
How are you getting the product out of the rb after the distillation?

I can't seem to get to the bottom of this process. People who know the process are being very hush hush about it.

I would plan to use heat and literally just pour it out.
 

flatslabs

Member
Chonksi:

Just look up a simple 250ml distillation apparatus, replace the liebig with a short path head. Get a consistent heating source, get a good vacuum source. Start practicing distilling simple things, salt water, etc.

Mind the laws in your state about what you are wanting to do. Just because you can order all this stuff freely off of the internet, doesn't mean its a good idea to do so. You may have good intentions, but other people that order this stuff don't necessarily.

I haven't checked the laws recently but i do recall in certain western states where methamphetamine is a problem that Erlenmeyer flasks are illegal to own. In Texas, there are a number of prohibited glassware items, etc.
 

flatslabs

Member
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.
 

Chonkski

Member
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.


Thank you so much for all the advice, I've been looking at a nice 19/22 setup, and also a short path head. Along with the stands etc.

And would one use a heating mantle for precise temp?

I will look up the laws of possessing or using equipment like this in ca, in the meantime does anyone know if I should not be getting into it around here? But I would love to just try some simple distillations with salt water like you suggested.

When it comes to cannabinoids, would I need a buffer of sorts to use instead of water? With a very high BP?

When it comes to fractionating, wouldn't you have to do this to separate the cannabinoids from the steam?


Edit: after seeing that it is not illegal to own a setup or distill water, but if it is being used for alcohol it is illegal to have without a commercial permit. They do have the right to sieze any equipment at any time without a permit as well.

Should one be worried about red flags or anything of the sort when ordering from ebay? The world we live in is pretty funny sometimes.
 
Last edited:

flatslabs

Member
Well, let me state again, I am not a chemist and it has been long years since I have dabbled in any of this stuff. I have done my fair share of vacuum distillations in the lab and have assisted on some complex reactions, but getting into too much detail I might not be able to answer.

Thank you so much for all the advice, I've been looking at a nice 19/22 setup, and also a short path head. Along with the stands etc.

Just look for a "19/22 chemistry kit" and you should get a few results. I see nice kits for 300 and under with more glass than you would need and a nice case to keep it all in.

And would one use a heating mantle for precise temp?
Thats one way to do it, but you need a mantle sized for your boiling flask. All you need to do is provide consistent temperatures on your flask. I remember using an oil bath (mineral or peanut?) on a hot plate for some reactions we did not have the right size mantles for, but all these dabs have my memory hazy.

I will look up the laws of possessing or using equipment like this in ca, in the meantime does anyone know if I should not be getting into it around here? But I would love to just try some simple distillations with salt water like you suggested.

Owning a lab distilling setup in cali is probably fine, its what you use it for which could be considered illegal. As GO Joe mentioned in the other thread, stuff like this could easily fall under several federal laws despite what your state says you can do, so just be careful is all, don't go posting youtube howtos.

When it comes to cannabinoids, would I need a buffer of sorts to use instead of water? With a very high BP?

I am sure there are several ways you can do it and me not being a chemist cannot answer those questions for you with certainty. I know Gray Wolf has a chart somewhere showing the boiling points of the different cannabinoids and terpenes. You could distill off all the bad stuff and leave the good stuff in your boiling flask for instance... But you have stated multiple times your goal is for solvent free, so what would you use as a buffer?

When it comes to fractionating, wouldn't you have to do this to separate the cannabinoids from the steam?

The best way to explain fractioning would be to look up some diagrams on how crude oil is processed into the various petroleum products, they have different boiling points so they capture them separately from the same process.

I think all you want to collect here to begin with is ThcA, the terpenes would have boiled off by then and there are no other fractions to collect that I know of, just collect all of the cannabinoids you want at once.
 

Chonkski

Member
Well, let me state again, I am not a chemist and it has been long years since I have dabbled in any of this stuff. I have done my fair share of vacuum distillations in the lab and have assisted on some complex reactions, but getting into too much detail I might not be able to answer.



Just look for a "19/22 chemistry kit" and you should get a few results. I see nice kits for 300 and under with more glass than you would need and a nice case to keep it all in.

Thats one way to do it, but you need a mantle sized for your boiling flask. All you need to do is provide consistent temperatures on your flask. I remember using an oil bath (mineral or peanut?) on a hot plate for some reactions we did not have the right size mantles for, but all these dabs have my memory hazy.



Owning a lab distilling setup in cali is probably fine, its what you use it for which could be considered illegal. As GO Joe mentioned in the other thread, stuff like this could easily fall under several federal laws despite what your state says you can do, so just be careful is all, don't go posting youtube howtos.



I am sure there are several ways you can do it and me not being a chemist cannot answer those questions for you with certainty. I know Gray Wolf has a chart somewhere showing the boiling points of the different cannabinoids and terpenes. You could distill off all the bad stuff and leave the good stuff in your boiling flask for instance... But you have stated multiple times your goal is for solvent free, so what would you use as a buffer?



The best way to explain fractioning would be to look up some diagrams on how crude oil is processed into the various petroleum products, they have different boiling points so they capture them separately from the same process.

I think all you want to collect here to begin with is ThcA, the terpenes would have boiled off by then and there are no other fractions to collect that I know of, just collect all of the cannabinoids you want at once.

Yes I'm am familiar with fractional distillation, I'm just a bit confused when it comes to collecting something with such a high BP. And JUST that compound..
 

flatslabs

Member
Is there anything with a higher boiling point in the starting solution which you want to get rid of? You aren't collecting just that compound, you are collecting all the low BP stuff, tossing that out. Collecting or leaving behind what you are after. Also keep in mind this whole thing is under vacuum, boiling points go down.

Heres a video showing how this works on a basic level, just instead of all the fancy cow and pear flasks he is using, you swap a regular clean one in when you need the fraction you want to collect. https://www.youtube.com/watch?v=L6BDHiJF2Dw

With that being said, I don't think there is much more I can contribute to this thread. I don't have the necessary gear or starting materials, so I wish luck to anyone who wants to attempt this.
 
Last edited:

Chonkski

Member
Is there anything with a higher boiling point in the starting solution which you want to get rid of? You aren't collecting just that compound, you are collecting all the low BP stuff, tossing that out. Collecting or leaving behind what you are after. Also keep in mind this whole thing is under vacuum, boiling points go down.
This was a nothing thing I was wondering, how much vacuum is this process under?

Perhaps what I want are the heaviest of compounds so I would be able to just leave it like you suggest. But if I were doing it that way, it wouldn't be steam distillation because I am using nothing in place of water, correct?

This whole time I've been picturing it as collecting the re condensed THC
Thoughts?
 

flatslabs

Member
The vacuum thing has been answered elsewhere already. And also as discussed, you use steam distillation when you are dealing with heat-sensitive organic stuff you don't want to break down, the steam lowers the boiling points of the compounds and provides a little bit of a "delivery vehicle" for the distillates.
 

Chonkski

Member
The vacuum thing has been answered elsewhere already. And also as discussed, you use steam distillation when you are dealing with heat-sensitive organic stuff you don't want to break down, the steam lowers the boiling points of the compounds and provides a little bit of a "delivery vehicle" for the distillates.

Haha, just about everything you have been telling me is already obvious. I am well aware of just about every point you made.

I appreciate the help very much, but you have just repeated all of the basics of this process over and over.

I am aware vacuum is needed. We haven't discussed what measurement would specifically be needed for THC.

I am aware that steam acts as a vehicle, which is why I brought up using a buffer other than water, water is not 'solvent free'.

No offense, but I feel offended.

Do you have any speculation at all on the refining process @Phate undergoes to achieve his steam distillation? Or are you just equal in spitballing here?
 

flatslabs

Member
Haha, just about everything you have been telling me is already obvious. I am well aware of just about every point you made.

I appreciate the help very much, but you have just repeated all of the basics of this process over and over.

Sorry man, I was just trying to help answer the questions you were asking. If you already know the answers, why do I keep repeating them?

I am aware vacuum is needed. We haven't discussed what measurement would specifically be needed for THC.

This has been discussed, go read the other thread, and is one of the reasons I am no longer pursuing this experiment

I am aware that steam acts as a vehicle, which is why I brought up using a buffer other than water, water is not 'solvent free'.

No offense, but I feel offended.

I am aware water is technically a solvent, but I don't think it qualifies one in the sense that we are referring to. I don't think they are testing for water in those residual tests, but you can always dry that out. I honestly didn't mean to offend.

Do you have any speculation at all on the refining process @Phate undergoes to achieve his steam distillation? Or are you just equal in spitballing here?

I have never heard of Phate until I came to this site, I don't get into all the Cali club politic stuff. This is a pretty basic process and I have had the idea in my head for several years as I am sure have several others. More recently, this article stirred my interest up: http://medicalmarijuana.com/sensi-social/forum/thread.cfm?artID=996
 

Chonkski

Member
Sorry man, I was just trying to help answer the questions you were asking. If you already know the answers, why do I keep repeating them?



This has been discussed, go read the other thread, and is one of the reasons I am no longer pursuing this experiment



I am aware water is technically a solvent, but I don't think it qualifies one in the sense that we are referring to. I don't think they are testing for water in those residual tests, but you can always dry that out. I honestly didn't mean to offend.



I have never heard of Phate until I came to this site, I don't get into all the Cali club politic stuff. This is a pretty basic process and I have had the idea in my head for several years as I am sure have several others. More recently, this article stirred my interest up: http://medicalmarijuana.com/sensi-social/forum/thread.cfm?artID=996


Well I appreciate your kindness and straightforwardness.

I suppose I just get a little anxious when I am hard at the drawing board of my own mind.

It's times like these I wish I could speak instead of type. I feel like too much gets lost when typing and reading. I have ADHD or something.

So after going back reading, I see that you are right. I must have missed it because I didn't fully understand the concept when you brought it up. I apologize.

When I bring up phate. I don't mean just him. I mean all of these solvent free extracts I see pooping up left and right. Videos on Instagram of kids no older than I of them pouring out golden honey with captions like "Str8 out da clear masheen #raw". When I just want to be able to experiment with the concept!

Like I said, I could litterally care less about the profit. I just have no patience in waiting for the cover to be blown..

Sorry for becoming a bit rantish for a moment. :tiphat:

And thank you for the resource. I'm going to read now
 
Top