Using Water to remove water Solubles

My distillation setup currently involves a 300mm vigreux column because that’s the kit I got :smile: Here is a picture from a few runs ago to give you a quick idea:

Because of this when I an stripping the Etoh out I am left with a very watery mix afterwards. I have a hydrometer on the way so I will be able to test my Etoh to know what % I’m recovering (to see if I have too much water content).

Long story short when recovering Etoh from a 2nd wash I noticed that some of the shit I extracted precipitates out of the water and forms globules. Using a stirbar seems to cause it to precipitate more quickly and then it spins out and sticks together and then they stick onto the sides some while the water is pulled out. I don’t have any pictures of this but I’m sure you’ve all seen water and the shit I extracted do the milky separation thing.

When I was running some 3rd wash (I do the 70/30 iso 3rd wash like skunkpharm) and evap’ing into air with a heat mat and ventilation I left the pyrex dish at an angle and the remaining water evaporated off in one spot of the pan.

When I tested (burned a small amount) the amber colored shit I extracted where the water evaporated it was mostly sugar and water solubles. The remaining shit I extracted (FSO?) was stronger and seemed to have less water solubles than normal. When I was trying to evaporate some of the water more quickly I transferred a small amount to a shot glass and when I tried to clean the shot glass later on 91% iso would not clean out the gunk on the bottom (likely water solubles).

I’m using the 3rd wash to make edibles with so the water solubles aren’t really an issue with this batch. It probably had more water than typical as some of the batch came from cleaning things (and left to open air some).

I’ve been wondering if this could be taken advantage of and used to refine the shit I extracted and remove water solubles. I have a few experiments planned but it will be a long time out as I’m an individual and not a business.

what exactly are you referring to as Distillate?

recovering alcohol off a wash is distilling your solvent. It is not producing what most in the cannabis industry refer to as distillate.

near as I can tell you’re referring to “crude”. which is the minimally processed output of a primary extraction. that extraction can be done with hydrocarbons, ethanol, CO2, or any appropriate solvent.

removing the primary extraction solvent via evaporation is standard. recapturing that solvent takes you from evaporation to distillation.

By definition: the “distillate” is that which evaporates from your boiling flask and condenses on the other side. ie your ethanol in this case.

to achieve what most in this industry call “distillate” (distilled cannabinoids), one has to achieve vacuum levels in the 1-300micron range (depending on equipment chosen) and temps in the 130-190C range in order to evaporate & then condense the cannabinoids.

it does not look like/or sound like you are doing that…

image

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here is a thread describing @Killa12345’s first attempt at “distillate”.

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Thanks for the definition. I guess I was referring to the shit I extracted. I’ll edit my post.

Sorry if I seem irritated but I figured somebody would comment on the dark color of my 3rd wash even though it has nothing to do with my post if anything it helps show the difference between that and the water solubles.

I guess if you are running short path then this is pretty pointless so maybe it doesn’t really make sense in this forum.

3rd pass with etoh doesn’t have to be that color. but usually is. because most folks doing cryo-ethanol would not use super cold on the third pass.

as for the water solubles, using water to remove them seems fairly logical. Except for the part where ethanol and water are miscible in each other.

louching the cannabinoids out of the etoh with water, then picking them up with something that is not miscible in etoh or water is an approach.

https://future4200.com/search?q=louche

I used straight RO water heated in a sep. Funnel to rescue some PG mixed crude I fucked up. It worked pretty good. I’ll know after my buddy @GrowingBalance207 runs it in his spd

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Now I’m even more confused.

You’re irritated because nobody diss’ed the color of your extract?

And wandering off because we all do SPD so your questions or insights are irrelevant?

Sorry Instagram and Facebook haven’t served you well. This place is different.

Learn how to search. Explore the data dump. Ask questions. Share answers.

Try not to let anyone ruffle your feathers. It’s seldom personal, and usually just someone in a hurry…

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Didn’t you ask for help on that one?

I had the same problem. I boiled off the water and diluted the little 6 gram test run with 500ml of 99% isolpropyl. Threw in a gram of activated carbon once i got it to about 75c (or whatever ISO boils at at my altitude), kept it there for 20 minutes, then filtered over a celite cake. Dark color was almost completely remediated, but it likely still has water solubles in it. I have the rest of my extract still in solution, so I’m going to do a liquid-liquid extraction to remove those water solubles. I thought about skipping that step, but I’m betting my cartridges will thank me if I don’t have sugars and other shit clogging up the coils.

I did indeed

I appreciated the definitions, I do plan on eventually trying SPD, and the explanation will help me communicate better. I’ve read a lot of posts and I searched on this topic a few times before I ever made the post. I had no idea it was called louching.

I don’t really do facebook and the only time I look at instagram is to see one of beaker’s posts. It’s hard to think that you didn’t expect to ruffle some feathers. It seems like a few of your posts are condescending and dismissive and you’ve gotten similar reactions a couple times. You know what you’re talking about and you do this for a living so I’m sure it is probably tiring seeing people doing things the wrong or using the wrong terms. You’ve done a lot to help the community and dozens (at least) have improved their runs based on your help.

@coppertop the dark color doesn’t bother me but if I can easily make it more potent then that’s what I’m after. I don’t know if I would try carbon for that reason but I do plan on trying some celite next time I winterize. I did winterize my 3rd wash, it was kind of funny because the dry ice actually caused the water to freeze out of the iso solid and it took forever for the rest to go through the buchner. Because the 3rd wash was room temp I think is why winterizing picked up so much stuff (filter looked nasty!). When I winterized my 1st and 2nd washes that were extracted frozen (~ -16 to -20 deg C for 4 days) the filters came out clean like they were out of the box. I used syringe filters (.22 micron ptfe) on the 1st wash and I could see the color lighten up and the filters certainly were getting clogged up.

It’s cool to know that louching is a useful strategy, maybe when I finish up my 3rd washes next time I will just get rid of the water off the top after the iso evaporates and see if it turns out any better.

Today I infused some butter with it and decarboxylated it. I did add a small amount of sunflower lecithin. I’m waiting for them to cool right now. The last batch I don’t think I decarb’d well enough, I was too worried about the high temperatures and my thermocouple seems to be off. I used a glass thermometer and an IR one this time which were both within about 1.5 deg C of each other, where the PID was reading +30 deg C (so I must have been under temp in my previous batch). This is the first time I saw the CO2 bubbles (thanks guys for that clue!).

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So your take is that I deliberately tried to piss you off, or cut you down? You’re certainly free to think that. However, that’s not how it went down.

I saw your post. it didn’t make sense. I asked clarifying questions, and gave you the pieces I thought you needed to improve your description to the point where you might get the discussion of using water to remove water solubles (from crude) that you were looking to initiate.

yeah, you’re right, a couple of folks have gotten their panties in a twist over my responses. that’s a couple (shit I’ll give you four or five if you need) out of hundreds of cogent responses. could I do better? maybe. Certainly I’d be less brusk if this was paying the bills.

You stated you were making distillate (yep, technically you were). Did you need me to correct you? No, but it seemed like it might up your game…more importantly, disambiguating here was going to be useful for those following behind you. If misinformation is allowed to stand, the signal to noise ratio here degrades.

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where was the probe for the PID located? if it is measuring the temp of your mantle (either internally to the mantle or between the mantle and the flask), it is not unusual to find the temperature different from the actual contents of the boiling flask. 30+C seems a little high and might be indicative of a problem with the calibration of your mantle.

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You helped me out and I hope at some point I can be helpful, too. My expertise lies in other areas. You have a good eye for safety and it helps people keep that in mind before they start mindlessly connecting and combining things. I hope you had a good turkey day if you are into that type of stuff, I kind of wasn’t looking forward to it this year but it ended up being pretty solid.

The PID thermocouple is taped with kapton tape to almost the bottom of the RBF or reaction chamber. I checked the temperature of that spot with an IR thermometer that I trust and the PID seemed to be way off. I also had the glass thermometer touching that spot (from the inside, but still shouldn’t be off by that much) Thinking back on some of my temp control problems I think this probably has been happening for a couple of runs. I should probably invest in a traceable thermometer since with the variac I’m really just using the PID as a thermometer anyhow. I sent the inkbird guys a message and they will tell me what I messed up or replace it; they stand by their 30$ PIDs pretty well.

The brownies came out good although I didn’t mix the cocoa powder well enough and every now and again you get a small chunk of cocoa :slight_smile: They are much stronger than the last batch I made and I tested a smaller square.

I remember making cookies when I was in high school and they were so strong it was almost like tripping. The crockpot must have happened to get hot enough to decarb that time because they were usually kind of weak. I think I’m gonna use my 3rd washes for edibles going forward. I’ll just save a few of them up over time and make up a big batch it will be easier to decarboxylate it that way.

I haven’t used many of the ink birds, I don’t recall them having much in the way of options. With more advanced units you can accidentally tell the screen to lie to you in several different manners.

Some have a fudge factor, many allow you to define the type of thermoprobe (incorrectly if you like), and I’ve hit at least one that didn’t tell the user if they were in f or c.

Auber are my current favs, although I used to shop at thermomart & omega really are the gold standard

I myself am getting bentonite to remove my water solubles as my try with carbon, heptane and water yielded a great looking end product, but or was more of a hassle than i thought it would be and stuff got lost in the emulsion layer. So the hassle of water washing lead me to want to try bentonite after hearing @TheLostBiologist mention it.

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you can break up water emulsions with a saturated salt (NaCl) solution, if you do liq/liq separations with aqueous layers its nice to have some ready for the inevitable recalcitrant emulsion

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the small trace remaining pg came out in the heads fraction before main body

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You mean to say that by increasing the polarity of the aqueous layer with NaCl, emulsions kinda go away?

Do you do this dropwise directly into your sep funnel?

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I use a 10% salt solution and the emulsion is definitely reduced in comparison to straight water.

However back in the day, before I worked with cannabis, I would use loads of salt to physically break emulsions up and knock them downwards. Then I realized increasing alkalinity was all I needed to rid of my emulsions.!

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