LLE second test

I made a previous post outlining a basic liquid to liquid extract method for removing terpenes. I noted that some more refinement and repeatability were needed. I needed to isolate the effects of LLE alone without other factors.

For me this month is ground breaking this way. For me it is a huge time and compound saver.

I dissolved the extract in methanol. Then I winterize and filter it. This month I was able to chill the methanol in a bath down to about -80C. I filtered as usual however more than just white wax got filtered this cold.

After filter I estimated the number of grams and doubled the amount of milliliters of hexane solvent for a 2:1 ratio. I poured the methanol into this and then began a series of water flushes with additions of small amounts of fresh methanol between. I catch all in a pot, saving the top hexane layer of cannabinoid. When the flushes began to run clear and want to make an emulsion I stopped.

The hexane was purged and then the compound decarboxylated under deep vacuum at a mantle setting of 125C. I was puzzled why the stir bar was having such trouble getting spun up. Lolz! Now I know. I sampled some med and there is zero terps. A no boil operation removed all the terps and compounds that thins this stuff normally. The stuff behaved like first run distillate but not decarbed. Wierd.

There are no waxes to speak of but the oil is still dark. Yet, smooth as anything I have smoked. Not potent like it will be when I do run it in distillation mode but my goodness just yanking the waxes out and washing the terps made something I can live with lol.

It is like potent good shatter but nearly zero flavor. Smooth smoke.

Here is the collection pan that captured the methanol, water, terpene flush. I freeze it so traces of compound will precipitate out. Very little was in there. These terps have never been cooked and they smell actually pretty good.

This is what it took volume wise to LLE out terps from about one ounce of concentrate. Total methanol used for dewax and de-terp about 250ml. This is easily recovered through distillation.


You da man! All of your posts are so interesting and you always manage to get me interested in trying new methods.

How do you feel about LLE vs DCVC for distillation prep in terms of ease and effectiveness?

LLE no question. Once the technique is down it takes just minutes. No clean up and no stationary phase. DCVC is not hard and can seperate most things but it takes many individual steps and time and clean up. This tech is just dumping in flasks of stuff in the right sequence and draining the bottom.

Just think of running your next batch of med in a distillaiton rig. It is the exact same except in addition to dewaxing there are zero terpenes AND the crude had never been boiled or above about 100C briefly to purge solvent. Otherwise the same.

What kind of purity could you pull out on a first pass?

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Did you add salt or modify the pH of the water at all?

No additions to the water. Just tap water.


I get zero purity on a first pass because I don’t have a distillation setup yet :frowning: the cost of rotary vane pump, pirani sensor and cryogenic sublimator have made the process unachievable for me atm. But I love learning and preparing for when I can afford the equip upgrade! As I will only be doing runs for personal meds I intend to pretty much copy your setup and process. You have made it look so appealing and rewarding. My current plan of processes is: crude> LLE> SPD and run 2 or 3 passes of SPD until adequate purity is achieved.

At a first glance your method above is fairly similar to a classic dewaxing tek but with the added step of extracting the THC/A from the methanol and into the hexane. So where do the terps go? Do they stay in the methanol? Also is your crude THCA or THC dominant? I noticed that you mention a decarb step which would make it seem obvious you have a THCA rich crude but for some reason I feel like in some of your other posts you worked with decarbed crude. I could very well be mistaken though

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I wonder if one could extract the terpenes out of that aqueous solution without destroying/degrading the terpenes?

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You can evaporate the aqeous layer off without heat, or without much heat then concentrate them in a number of ways if you wish. The problem is that this LLE also removes significant gums so you would need to seperate those in a seperate process. Probably extract them with hexane. I think the recovery of the terps might be spendy resource wise compared with buying already isolated terps but I see no reason why not.


Try freezing the aqueous layer and pouring off the terps


@GlassAlchemist this was what we were talking about.