Yes you can definitely do that, but why?
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@square_root_pharms was speaking of 1 solvent for everything two post above. I figured do it as I stated before with methanol (why not)? I remember speaking to you at glg northern cali Meet up about reproofing ethonal and you to recommended I should look into methanol…
Every solvent has its place
Probably a low cost decent way to make distillate on small to medium scale.
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Thanks
I’ve done 0c methanol extraction before.
You end up with a ton of browns and greens and more sugars. So either an LLE or a louche is in order after winterizing.
You’ll need to get a bunch of powders involved but I’ve made nice first pass 90% distillate from a methanol base. So it’s totally doable.
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Sweet! Thanks for the input! May I ask your preferred method now?
You lle into heptane?
Depends on my desired end product.
I was most recently doing 0c ethanol with some charcoal
Then either
A) concentrate with RO membrane then louche into pentane
Or if you don’t have a membrane I run a spray fuge to a 70-80% saturated ethanol solution (about 1lb per litre) then
B) Louche directly into pentane.
After that, I’d CRC under pressure if going into shatter/etc. Otherwise I’d just concentrate and distill it, catching terps. Then distilling the cannabanoids
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Thanks for sharing
Hey Everyone,
I found something recently worth discussing here. Seems you can do a near room temp winterization in an hour by using two solvents. Do a bulk extraction with Isopropyl, reduce it to oil, then rehydrate it with 95% Ethanol, you start seeing immediate wax formations at room temperature. I believe this is due to Ethanol’s higher polarity.
By placing this small amount of alcohol in the freezer and you get lots of waxes within an hour. Going further, use a little dry ice alcohol bath to reach -60f and you can have very solid waxes in the same time. The bowl of waxes you see below is sitting in a bowl of ice water.
The filtering can be as simple as pouring this through a paper napkin in the freezer. here’s a few images of just that.
Your thoughts?
…Mimi
Pictures:
#1 Bowl with ethanol and waxes.
#2 Light colored waxes in napkin filter.
I set this napkin in a funnel in the freezer so it remains frozen during the filtering. Whats interesting is, letting this sit out for 24hrs. The wax stays solid as it heats up to room temp. Even after 24 hrs, the waxes are still there, though shriveled up after the alcohol evaporates.
#3 Dark colored waxes in napkin filter.
The longer you let the waxes crystalize, the darker it becomes, so I think longer freezes might cause more cannabinoid losses. This is a 4 hour stay in the freezer.
This is where analytics come in handy.
You have access to a GC now yes?
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Yes. But I’m trying to get my head around all the issues. Besides potency what other tests would characterize this for you?
You have “waxes”….are there cannabinoids there?!?
ALL you have access to is “potency”. So it’s about how you ask the question.
How much did I start with?
Where did it go?
Is there any in THIS waste stream?
How much?
Can I change that? (Longer soak?!?)
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Hey Cyclopath,
I did ask those questions this past month in an update to graywolf. Here’s a .PDF version of that email with all the test results. That’s a bit off point to the question I posed here about what am i seeing in Rapid Winterization. All three tests used Rapid Winterization on each jar (8 jars) with the above pictures showing the waxes produced.
I will run another test to compare winterizing 4oz of hemp the traditional way, and now with Rapid Winterization. This will answer the question on efficacy.
Anything else I should be considering?
Email-RSO 2.0 Update - GW 02-08-2022.pdf (595.8 KB)
Hey Cyclopath,
I ended that last reply with a question regarding that .PDF, not the main reason I posted this morning, let me get this back on track.
Basically, what I want to know is if two solvents with different polarities caused near room temp wax formation. The waxes start forming as the warm ethanol cools. At room temp you can see this happen. Placing the bowl in the freezer for an hour finishes the wax crystallization. Longer freezes just turn the wax a darker green, probably with more cannabinoids. (thats easy to prove in testing)
So, does extracting with Isopropyl, removing the Isopropyl, then dissolving these less polar resins with higher polarity Ethanol really setup this room temperature winterization? That .PDF shows the volumes of plant, alcohol and times if anyone wants to give it a try.
I’m failing to see where and why there is any confusion here.
You’ve (re)discovered that Isopropyl seems to extract at least one type of compound that is not soluble in Ethanol at most reasonable temperatures. I’m pretty sure I’ve seen mention of that effect somewhere else on here, possibly above in this very thread.
It’s also why many ethanol extractors run very cold - if you’re at -60°, ethanol is not going to be very enthusiastic about dissolving any lipid type compounds.
Is this due to the polarity of ethanol relative to isopropyl? Polarity affects a great many things, and seems to be an important factor in much of our work, but I’ll let someone with chemistry training chime in on that one.
If you were to extract with isopropyl, remove the solvent, dissolve it in ethanol, chill, filter, recover the ethanol, and do the same procedure with methanol, I’d be willing to bet that you would find even more compounds falling out.
Do it again, and dissolve in some other solvent, and you may find yet more compounds that fall out or don’t dissolve in the new solvent.
As you’ve discovered, changing the temperature of your solvent may have a similar effect.
It is possible that water-washing your crude before dissolving it in ethanol could remove a bunch of your undesirable water-soluble compounds and improve your finished product.
Modifying your water wash with the addition of salt - which salt? Start with good ol table salt and explore outwards from there … - may change what happens once again.
Thank you for your input.
You’ve (re)discovered that Isopropyl seems to…
True. I tell people I haven’t found a diamond in the rough, I found a diamond in a parking lot. This area of chemistry is well travelled…
Is this due to the polarity of ethanol relative to isopropyl? Polarity affects a great many things, and seems to be an important factor in much of our work, but I’ll let someone with chemistry training chime in on that one.
Thats what I’m hoping for. Not so confused, but not being a chemist, I’m looking for confirmation that my theory is correct.
If you were to extract with isopropyl, remove the solvent, dissolve it in ethanol, chill, filter, recover the ethanol, and do the same procedure with methanol, I’d be willing to bet that you would find even more compounds falling out.
HAHAHAHA. The Methanol arrived yesterday, testing to commence. Its good for testing, but not so much for home MMJ patients. More to come later…
>As you’ve discovered, changing the temperature of your solvent may have a similar effect.
Solubility decreases with decreasing temps. I do observe that here in the solution. It starts by forming wine veins on the side of the bowl then forming waxes.
It is possible that water-washing your crude before dissolving it in ethanol could remove a bunch of your undesirable water-soluble compounds and improve your finished product.
Actually, my process does do that. I add saturated brine water to salt-out the Isopropyl which causing phospholipids to immediately fall out. Here’s the video -
I call this whole step ‘Silting’ as it also cleans out water solubles, trichome shells with the phospholipids. This new step removes the polar and semi-polar compounds leaving a richer non-polar base once reduced (My tests in the above .PDF show that is not necessary, but still beneficial for the Rapid Winterization). The control jars were a straight wash in Isopropyl, reduced to oil, then re-dissolved in warm ethanol. Once the ethanol starts cooling is when you see waxes form. So, Silting with its brine wash helps by removing the polar stuff, leaving condensed non-polar lipids.
Another question I have is this. Do non-polar lipids have varying degrees of polarity? I envision Isopropyl, being less polar, collects non-polar lipids that Ethanol cant touch because of it’s higher polarity. I haven’t seen an analysis showing a range of polarity with lipids.
Modifying your water wash with the addition of salt - which salt? Start with good ol table salt and explore outwards from there … - may change what happens once again.
I have been using table salt with and without anti-caking compounds. Also Kosher, Pickling and ice cream salt without anti-caking compounds work. It’s the same sodium chloride packed differently for different uses. You can salt-out Ethanol with Potassium Chloride but it spikes the pH up to 12 introducing a whole set of other problems.
Oh, the other part of Rapid Winterization is the volume of alcohol is vastly reduced, therefore requires less time to freeze. 1 oz of oil would take 280ml for a 10:1 ratio, just over a cup. The time required for freezing is now substantially lower. I can take 2 oz hemp and have refined winterized finished oil in 2 hours, instead of 24 hours. The distilling time dictates the overall time. The wash, Silting, winterizing, and final reduction are all very fast.
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Here’s something funny. I used ChatGPT to explore the different types of salt. Seems Magnesium Chloride might be a good, but more expensive, solution for salting-out Isopropyl.
2023-02-24 Type of Salts.pdf (48.8 KB)
You are aware that chatgpt is only trained on how to CHAT?
It will happily make shit up…,
Useful tool, but it’s responses need to be taken with…you guessed it…a grain of salt.
And priming it with nonsense (Various sodium chloride salts have different properties.) won’t help.
Q: 4 of those are not salt! why did you list them?
Because I’m a #%%^%?! Chat bot who knows nothing but how to string words into sentences. I made shit up because I thought you wanted me to…
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ChatGPT does frequently spot out nonsense. It has no knowledge, it is just a word generator.
However, sometimes it can be useful as a research summarization tool. I’ve never played with salting things out of aqueous/alcohol solutions, so I’m interested to see where this exploration leads.
Unless of course someone who has been down this particular path feels like shining a light on any presently unseen traps?
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If interrogated/primed correctly…
@MimiEmu over here we have an example of chatgpt fabricating a citation…
I only verified the first Mg salt vendor. Have you verified the rest, or looked into what percentage Mg they offer?