Could it be lipids in the CBD? Phosphoric acid reaction

What a weird fucking texture, like thick snot. Guessing it’s not supposed to be? Could it be lipids in the CBD? I’ve put 20g isolate in 50ml methanol in the freezer to see what happens.

Phosphoric acid reaction


You shook it too hard.

Use a phase contactor.

Did you neutralize with bicarbonate?

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Um excuse me, you said and I listened:

Well, actually I’m not sure how to link to another thread but ill paraphrase:

“Shake that bitch like it owes you money”. -@Rowan

Did I expect too much in interest?


Here’s the specs:

Prepared 500ml 5% bicarbonate (25g to 500ml DI water)
Prepared 500ml sodium solution (unmeasured, water softener salt)
Prepared 20g CBD isolate
Prepared 40g 99% iso
Prepared 4g 85% phosphoric acid

Applied heat to all glassware to dry using a heat gun.
Filled boiling flask with argon for about 15-20 seconds. (I understand this isn’t enough, but I only have a calibration cylinder until Monday)
Combined CBD, ISO and acid, added solution to boiling flask, setup for reflux.

Used the wrong condenser at the time, refluxed for about 3 hours before allowing the solution to come down to room temperature.

Transferred solution to graduated cylinder for measurement, 30ml~.
Added solution to sep funnel and washed as follows:

  1. 30ml pure water, no shake, 30+ minutes
  2. 30ml 5% bicarb, no shake, 30+ minutes
  3. 30ml 5% bicarb, remembered the shake it, 20 minutes or so
  4. 30ml 5% bicarb, remembered to shake the ever living piss out of it, also stirred with glass rod, 20 minutes
  5. 30ml sodium solution, shake + stir, 30 minutes
  6. 30ml pure water, shake, 30 minutes.

That’s about where I am now.

I’d like to understand how I went wrong here. Would never have occurred to me to consider I could be shaking it too hard.

I’m sorry to ask, but what is this? Google leads me to electrical shit and theres nothing leading me to an answer that I could find with that term here on f4200.

Should the shaking be a more, light mixing back and forth type mixing? Rather than shaking the funnel like a champagne bottle at a christening?

I’ll do another run today and I’d like to try to do it better. This is what I have to work on this run, I’d appreciate any insights on anything else I might have overlooked or performed incorrect in the process outlined above.

Next run proposed improvements:

  • Shake/stir for each separation phase
  • shake it like it owes me less money and I’m running a charity
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Came in this morning to find the separation like this :joy:


Try pouring off into a larger vessel and adding more of each of the constituent solvents until the layers separate again. Then use the sep funnel to clear those. You could also add brine to it first to see if that breaks up what’s going on in there. If all else fails try heat to increase the solubility of whatever it is.


Should I be doing a large ratio of brine/bicarb/water during the wash rather than 1:1 as general matter of practice?

I guess I’d like to know, can I avoid this entirely by not shaking so hard?

I pulled the CBD in methanol i put in the freezer last night, looks clear to me; so I’m thinking it was my process.

As far as the brine wash goes, are you guys measuring to a specific concentration (I’ve seen 10% mentioned elsewhere) as I’ve seen it done a few ways (by percentage, and another mentioned just adding salt until it was super saturated.

Most labs I’ve worked with had a saturated brine sol on hand. It was made this way and always had solid salt on the bottom of the bottle.

Give the funnel a few inversions, opening up upside down to release any built up pressure and closing before giving it a few more shakes. Some things hate each other and separate well, no matter how hard you shake. Others you have to find the sweet spot between cleaning your layer and doing whatever you did, i’d like to call it an emulsion but i really don’t know.


This was my first thought as well.

I’ll give this a try today and see how it differs in the outcome.

I don’t know if I’m going to play with this too much today, but I think it would be a good exercise to figure out how to clean it up. .

Really appreciate your input @NewLevelProcess

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You have hit your pka range and have made some of the cannabinoid in a water soluble limbo… most likely need to add some acidic water


Would you mind explaining how you came to that conclusion? Trying to learn.

Might that explain this oddness?

Your top layer has all of your cannabinoids but has no solvent so it is very thick like snot. Try adding some heptane after or with step one. Or if you still have your first batch of snot… Add heptane to that and you should see decent separation.

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This might be an ignorant question, but did the solvent (ISO) wash out with the aqueous layer?

Am I understanding the purpose of this correctly? The cannabinoids have a greater affinity for the heptane and would migrate to that layer (not all at once).

So are we still on the idea that there was too much shaking during the washes? I’ve got another 20g reaction going and right now that’s the biggest change I have planned, per @NewLevelProcess, to invert a few times per wash, evacuating the pressure via stop cock while inverted; rather than shaking the bejesus out of it

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O I didn’t realize you still had it in iso. Yes add heptane and the cannabinoid will go into the heptane layer and the iso will wash out in the water


Okay, so the solvent did all run out with the water and left me with this glob of… ‘oil’?

Is Heptane absolutely required to make this work? I have it, bought it just in case, but I’m trying to limit the number of solvents I have to expose myself to if at all possible.

I guess this opens up some new thoughts and questions. My initial plan was after the water washing to move the remaining ‘crude’ to a boiling flask and try to distill. It seems I’m not out of line to think I needed to added it back to ISO considering it’s current condition. My goal with this step was purification.

I know LLE is another kind of purification, and if this process requires doing LLE to get it out of solution and into distillation or chromatography, how might I change the process above?

Heptane (in equal amounts? To solution, 30ml in above examples) to the first, non-neutralized wash per @Biscuits? I’m assuming as I drain the aqueous layer, and add in brine or bicarb solution that it is changing the environment (ph or otherwise) and allowing more cannabinoids to move over to the heptane layer?

Yes, 100% you need something that combine with water (heptane/alkane) as all of your isopropyl is mixed with your water


Thank you. Would 1:1 heptane be a good starting point? Currently thinking something like this:

Assuming about 30ml out of the boiling flask.

Combine 30ml reaction solution, 30 ml pure water, 30ml heptane. Invert 10 times releasing gas every other inversion or so. Allow to separate 30 minutes. Drain aqueous layer. Repeat with: 3x 5% bicarb, 1x saturated sodium solution, 1x pure water.

At this point I expect I’ll have a heptane layer containing the cannabinoids and whatever else is miscible in heptane.

In the opinion of anyone reading this, would the heptane solution after solvent has evaporated be safe enough for your personal consumption? @Killa12345 not withstanding :heart:

My plan is and was to move the crude solution to SPD/DCVC processes next

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3-4ml of heptane per g of cbd


Thank you, I’ll plan on 60-80ml heptane and see what happens! Will report back later.

Polarity, surface tension , tempurature

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Getting somewhere!

I’m not sure exactly what I made but it’s pretty! Still needs to go through distillation or something. I’m guessing it’s largely d8 from its cold honey like texture consistency at room temp