Any SOP on terpene extraction ?


#21

@Thetetraguy: something like this? only with Vac?

image

which strangely, when I asked the all knowing one to “show me!”, actually pointed at something larger…

shhh! don’t tell anyone :shushing_face:


#22

Yup just like that. Instead the dropper attachment that doesn’t work with vac, I use a 100ml seperatory funnel as my recieving flask. After each flask swap i bleed the water out into a bigger seperatory funnel that ends up catching another ml or two from the residual in the water after 4 or 5 runs. At that point I also replace the water below, I should be boiling the water separately then injecting the steam so that the boiling water doesn’t ever get any drippings from above, which only happens if u let it cool before taking it off.

If i had more time and money I would like to incorporate a centrifuge that would have a camera to see the liquid/terpene line while it’s spinning. What I haven’t figured out is how I could inject new terpene water while being able to pull water out from the “bottom” periodically. It would also be neat if it was jacketed so u could get it really cold. I just can’t wrap my head around how liquid lines would work with something spinning so fast and continuously while being medical grade.
That would make for instant separation and really quick retrieval, because I’m sure I waste 10% of it to glass contact alone.


#23

Ah, you need this! https://rover.ebay.com/rover/0/0/0?mpre=https%3A%2F%2Fwww.ebay.com%2Fulk%2Fitm%2F273338027194


#24

Makes sense to pull vac on a steam distillation setup to keep the water in the gas phase at around 60C. But has anyone pulled it off successfully? Seems like there are lots of dissatisfied terpene extractors here, but on the market I’m seeing lots of terp based products. Are the big guys hoarding the tech, or are they just lying? I’m using foreign reintroduced terps and people keep telling me how my carts taste better than anything on the market. The big commercial carts that say they have cannabis terps added back all either taste like steamed carrots or taste like they cheated and added back some foreign d-limonene along with the cannabis terps.


#25

Let me get this straight.

it puts D-lime in the distillate, mix 'em both together?
it puts D-lime in the distillate, and vape em all up?


#26

I said, doctor! Do you hear my belly ache?..we could go all day…


#27

For the hacked up microwave, is it important for male operators to wear lead shielded jock straps if they have not yet fathered any children but want to?


#28

@cannabuilder: what if you don’t dry it after steaming? Just freeze with LiqN2, and reduce to 1/4" minus by running through a screen?

What temp are you running your solvent? Would colder do anything to address the gums? What would an inline degumming look like?

Where's that degumming thread, Future?

I suspect the right solution might involve placing a bubble hash rig in front of the process. you’d probably want to run it longer that most folks do.


#29

Temp didn’t seem to have an effect on the gums coming out in extraction, we didn’t let it get any warmer than -40C. There’s something about introducing all that water and steam to the material that really made it want to release every molecule pf phosphatide into the extraction.

We’re filtering down to 0.5um after extraction so it’s in the solution. They first start to precipitate out during ethanol recovery (in a rotovap, thank goodness we don’t have to keep cleaning it out of a falling film). We’ll strain it again before going into the wiped film still, then more will precipitate out while it’s heated in the feed tank AND then it cakes up in the still body and grinds away at the wipers. No fun.

A hexane/saline wash will remove a lot, but not all of it, and it takes a number of washes to get there. We’re working on a citric acid SOP, we’ve just never had to deal with it in our process before so it’s new to us.

You’ve got some interesting suggestions we can consider playing with. We’re still waiting for the Milestone microwave system to come and to play with it. We’re cautiously optimistic that we won’t run into the same issue since we’re not adding more water to the process, it’s only steaming out what’s inside the cell walls.


#30

@cannabuilder

I have looked at the Milestone system in the past and am very curious to know how it performs with cannabis. At the time I spoke with them they didn’t have much to offer with regards to successful stories within the cannabis industry. If you wouldn’t mind sharing your results and thoughts back here or in a new thread I would be very interested to see what you get and your thoughts, if you don’t mind.


#31

The milestone system comes with standard 24 40 fittings, and you can sweep with nitrogen instead perhaps. Idk. Their rep wasnt able to comment on that idea.

@Future any comment on that?
Also what did u mean (future) when you said you distill HT pour offs? Is that just for solvent or do you actually distill the terpz?


#32

I’ve received some promising test data from one of the rep that I’ve compared it to my own. I can report back as soon as I have some hands on experience. Be patient and I’ll let you know when I do.


#33

Can you elaborate on the system used to achieve this @Future (DIY rig or something like the Milestone)?


#34

@Shadownaught I saw your instagram post with terpenes extracted via MHD. Did you use the Milestone system?


#35

Try this maybe; we did and it’s worth further experimentation. Yield wasn’t the best, but the steps need to be dialed in:

  1. Carry out hydrocarbon based extraction. Preferably use very cold solvent and with a decent amount of propane into it to capture more terpenes. Good input material is a must.

  2. Go through recovery and purge off the solvent at low temps. We use 20°C. Prepare to purge oleoresin in a vacuum oven.

  3. Use a slow release of nitrogen into the vacuum oven as you drop the vacuum slowly to match the release of solvent from the oil.

  4. Once the material is purged in the vacuum oven, move over to a short path distillation. Using a deep vacuum, low temperatures (not sure on exact temp), and high rpm on your stir plate, capture the first fraction from your oil. Make sure temps are cold on the condenser and that your cold trap is clean and set up with dry ice to assist in condensing the terpenes.

We tried this and the fraction smelt terrible immediately after distilling. The following day, the terpene fraction smelt exactly like WiFi OG which is what we pulled it from. It took a day or so to off gas whatever was causing the off smell, but now it’s great.

This method is worth trying again to see about dialing it in. The first try we used a diaphragm pump, but next time we are going to use our Ed30 to get a lower vacuum.

Maybe nitrogen comes into play on this @Future
@Noperuiy @skankhunt420


#36

Like @FRESHcoastextracts said his method is worth messing around with. We have done the same we set vac at 200 torr, you can look up the boiling points using a boiling point calculator by plugging in the vacuum pressure you are running. I believe we used Sigma eldritch. Set your condenser at 0ºC if i recall correctly.


#37

The terms “activate Terpenes”? I’ve never heard of this can someone explain?


#38

Gentle heat will allow terpenes to move towards the top layer of your solution or biomass making them more available to distill.

It’s nothing fancy we are just dealing with something that oxidizes and evaporates quickly so we must find a way to “activate” or move the terpenes to the top without degrading the target product.


#39

Ok, when you use the term activate it’s misleading. Cannabinoids more specifically THC is activated. What your talking about is In my words and opinion only, is stripping the plant matter of it’s terpenes. As far as “to the top” also is a little misleading. As they do reach the top of the still head, your correct, the do end up on top of the aquacious phase in the end. As far as degradation, I find that steam is very effective in proper removal though lots of peeps here will say otherwise. What is not good and causes color and funk too the end essential oil is direct contact of your biomass with liquid water. I know this is hard too understand but if actual hot or boiling water touches biomass you will get yellow and brown terps as a result. Dry steam if you will won’t cause this. For what it’s worth that’s my synopsis.


#41

Is that 200g of terpenes in 5 hours? Also, is that 3-4% of biomass or crude?