Isolating Cannabis Terpenes, Part II: Actual Process

[WaterFarmFan]

Hey hash head. Initially I thought as you about adding water to material before starting, but as I have come to understand with practical experience, h20 is very difficult to purge from material under vacuum at lower temps. By adding water, you are only making the process take longer.

I use a separatory funnel chilled to ~2C for several hours to separate terpenes from hydrosol. Terpenes ("alcohols, ethers, aldehydes, ketones, and esters" - GreyWolf) and other organics are not all crystal clear when they interact I would imagine. I want a full spectrum extract that takes the best of elite flowers and concentrates it even further. If that is a cloudy extract, so be it. I could care less if others make a clear extract (often using inferior trim) that is devoid of soul and character.

WFF

 

[Humpi]

WFF, have you tried blue river terps? or terps from companies like true terpenes ?

B

 

[hash head]

Hey hash head. Initially I thought as you about adding water to material before starting, but as I have come to understand with practical experience, h20 is very difficult to purge from material under vacuum at lower temps. By adding water, you are only making the process take longer.


WFF

maybe if it takes a little more heat might still be shorter length of time once you get that water distilling.. might not mess the terps up too bad as long as you don't get TOO hot

 

[WaterFarmFan]

Hey Hash Head. I am in the process of adding new pressure regulating components to my heated nitrogen back fill, and I will be adding some very detailed posts after that. I will say that I now think this process only makes sense using fresh flowers, which I freeze with liquid nitrogen and crush to hash consistency. More soon...

WFF

 

[pahval]

amazing work mate... im definetly trying this in future... may i recommend visiting future4200 forum, guys there are pros of extractions, maybe you can find something you want to add/youre missing... i hope youll benefit from it... btw absinthe gets cloudy when in contact with water because of the anise inside, try adding water to vodka, nothing happens...

 

[pahval]

hey WFF, ive been researching your setup for last couple of days, amazing work mate, i think you cracked the code, this has a potential to be standard diy equipment as hash bags are, i have some questions, i hope youll read this since it is 3 years old thread, as i understand, you are using vacuum oven in series with condenser and cold traps, you use nitrogen to bring up the temperature and to move terpenes that evaporate from buds trough your cold traps, i am wondering:


1. why then using vacuum oven? since its purpose is to heat up material, and you use nitrogen for that, would in your experience vacuum chamber be a good replacement of vacuum oven? (i come from overseas so there is no easily available equipment here, im trying to ghetto it all the way, i see the benefit of having material spreaded on a pan instead of in a pot as Pangea did it, but i tought of making simple vacuum chamber instead of oven, and using PID controlled heater of nitrogen to thaw the material)


2. as i understood, vacuum oven heats up material trough the plates material is on, since there is no heat transfer trough air in vacuum, what is the temperature you run your oven at? does your nitrogen follow the temperature of oven, or do you set your oven at xy temp, and then introduce heaten nitrogen?


peace...

 

[WaterFarmFan]

amazing work mate... im definetly trying this in future... may i recommend visiting future4200 forum, guys there are pros of extractions, maybe you can find something you want to add/youre missing... i hope youll benefit from it... btw absinthe gets cloudy when in contact with water because of the anise inside, try adding water to vodka, nothing happens...

Thanks for the kind words. Don't post much these days, on here or future, but I have spent 100's of hours over there reading. Not a great resource for growing, but some serious extraction knowledge.

hey WFF, ive been researching your setup for last couple of days, amazing work mate, i think you cracked the code, this has a potential to be standard diy equipment as hash bags are, i have some questions, i hope youll read this since it is 3 years old thread, as i understand, you are using vacuum oven in series with condenser and cold traps, you use nitrogen to bring up the temperature and to move terpenes that evaporate from buds trough your cold traps, i am wondering:

1. why then using vacuum oven? since its purpose is to heat up material, and you use nitrogen for that, would in your experience vacuum chamber be a good replacement of vacuum oven? (i come from overseas so there is no easily available equipment here, im trying to ghetto it all the way, i see the benefit of having material spreaded on a pan instead of in a pot as Pangea did it, but i tought of making simple vacuum chamber instead of oven, and using PID controlled heater of nitrogen to thaw the material)

I used a vacuum oven because I already had one to be honest. The main advantage is that it can assist in bringing plates and material to temperature before pulling vacuum. It is stainless/inert and also has the plumbing for nitrogen assist and vacuum line in addition to being reinforced.

There is a good current thread on future about the pressure dangers associated with nitrogen assist. The main point being that you need pressure relief values in case of overpressure, which could cause components to explode. I was reckless in using liquid nitrogen (without PRVs) in my oven and lucky that I was not seriously hurt or killed.

2. as i understood, vacuum oven heats up material trough the plates material is on, since there is no heat transfer trough air in vacuum, what is the temperature you run your oven at? does your nitrogen follow the temperature of oven, or do you set your oven at xy temp, and then introduce heaten nitrogen?

That was indeed the logic, but I do not think I ever got the nitrogen hot enough to really volatilize the terpenes in trichome shell. I really have no exact xy temps, but I think you could push temps up on both to 120C range.

It has been several years since I engaged in these experiments, but if I was going to do this again, I would 100% be using microwave technology instead of a vacuum oven. The terpene extraction setup would be largely identical except the material (likely fresh frozen ln2 hash) would go into a glass reactor that is housed in a chopped up microwave.

Here are a few relevant links that I think are helpful to the microwave tech:

https://www.hindawi.com/journals/ijce/2018/2957194/

https://future4200.com/uploads/short-url/ihAM7uw1LqIkA7j5c3NOW6LCjnq.pdf

https://onlinelibrary.wiley.com/doi/full/10.1002/tcr.201800045

This company seems to have a bunch of patents in the space:

https://www.milestonesrl.com/products/microwave-extraction-for-processors/ethos-x-for-cannabis

Happy to answer questions that I can.

WFF

 

[WaterFarmFan]

Pangea - What are your current thoughts on best practices for small to medium scale terpene extraction???