Methanol Crystals? What are these?

Hey,
I did a chilled ethanol extract. After evapping I then room temp winterized 4:1 in methanol while spinning with some charcoal.

I filtered over alumina and then started to rotavap the methanol off. I noticed some weird stuff on the inside of my flasks. Looks kinda crystally? Can’t get it out without solvent so not sure how to test.

Didn’t think methanol would drop anything out like this either, especially under heat.

Anyone ever got wee crystals like these?

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Maybe fats? Menthol is a solvent that coagulates fats in room temp.

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I figured the alumina + filter papers + celite would catch any fats along the way, but obviously could be wrong.

Celite stops the fines, not fats. Reason why its the 1st bed in your filtration setup. AO stops fats/lipids at freezer temps.

My rotovap flask looked just like that. I thought i had diamonds, seemed to be just bs and not worth scavenging from the flask.

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People seem to be doing well on the room temp methanol. This was my first go at it. Had a lot of gunk on top of the alumina bed.

You think it’s probably the fats in the flask then?

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If your waxes have preciptated from the solution then the celite will definitely grab the fats. In the case of methanol, the waxes preciptate at room temperature and the viscous oily components drop out of the solution when you chill the methanol.

Could be that when you transferred the methanol to that flask the solution was warmer than it is now and so now that its back to room temp its dropping small amounts of waxes from the solution. @tweedledew

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I think that makes sense.

So I guess you need to chill methanol for winterizing as well?

You certainly need to for stability purposes after you remove all those waxes. If i only use methanol for a warm dewax then the slabs always come out tacky at the very least.

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Good to know, I’m just going into distillate. I guess we’ll see how this run turns out :slight_smile:

What solvent dissolves these crystals?

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Why are you making methanol slabs?

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Hmmm, probably only get one shot at it since there’s not much there. Anything you suggest?

Because i smoke what i make and slabs are easy to produce and deal with. Methanol can make some real glassy shatter.

I know om removing the methanol to safe levels anyhow, i add ethanol to the mix after ive evaporsted most of it.

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Is it soluble in water? Could be sugars

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If it’s fats it will dissolve in hexane. I suspect it may not. I suspect it may be polar contaminants.

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10.1002@aic.11258.pdf (313.1 KB)

I found this to be pretty interesting so i thought i would share because someone suggested it was some kind of sugar.

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Yeah I’m just curious, I’ve done this process 100x with cold ethanol winterizing, never had issues come up. I’m guessing the warm temps had something to do with it

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As long as you didnt extract the plant material with warm ethanol i doubt you picked up as much sugars as what we see in the photos. My guess is that its some kind of lipid

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Test its boiling point? If you dont have solvents for solubility test…

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There’s like 1-2g scattered between 2 flasks :stuck_out_tongue: I’ll probably try heptane tomorrow

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