Whats this weird aqueous layer?

#1

Heyo!

Just winterized some butane extracted stuff in methanol. Took off a whole pile of wax and fats.
Roto-d the methanol at 65c under 25" vacuum for a while. Until only the occasional drip was coming off.

Poured it off into a jar and this happened.

Not sure what the top layer is… I wouldn’t assume water because I’d assume it would stay in solution (unless it’s alot of water and the methanol is mostly all gone? But by volume I’d assume there’s still 200ml of methanol). Also wouldn’t think it’s butane since it would’ve boiled off long ago. Maybe some oils or fats?

Any thoughts?

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#2

Did you freeze the solution after adding the methanol or just a room temp winterization?

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#3

Twas frozen overnight 6:1

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#4

Also it seems to be growing ever so slowly…

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#5

Hmmm… Does it feel slick/greasy or more “sticky” like water? Did you filter it through media or simply pour off the solution from the waxes? Did you add T5 or alumina to the solution before freezing?

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#6

Didn’t add t5 or alumina.
Ran it over a 7micron filter paper.

I’d describe it to be kinda in-between watery and oily lol
It also gets my fingers fairly sticky (but certainly less-so than a saturated cannabinoid solution would).

It’s just going into a distillate batch, so I’ll probably just suck off that layer and play with it when I’m bored one day :stuck_out_tongue:

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#7

Suck iT off bring to a boil and read boiling point Gives a hint to what iT. Is
I think water

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#8

I thought methanol would float on water so if this layer were water, wouldn’t it be on the bottom??

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#9

Methanol and water mix easily
And saturated oil is often heavier than water
One Could also drop iT in the freezer and see If iT freezes
It Will only freeze If less than 20 % is methanol

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#10

What temp was it winterized at?

And by overnight do you mean 8 hours, 12 hours?

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#11

You didnt do any ph stuff?

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#12

16h overnight in methanol. -18c freezer?

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#13

No pH stuff

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#14

When you chilled the methanol was the container covered? I cant think of a single reason why you would see that top layer forming other than water being present. Try adding some fresh methanol and a shit ton of magnesium sulfate, if its water it will get absorbed by the mgso4 if it’s not water then no harm you can just filter your solution.

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#15

I don’t believe that that’s long enough for that temp.

For example we do 24h @ -70, which is what is generally recommended. If your going to winterize at that high of a temp you will need to significantly lengthen the time.

My guess is the layer is fats/lipids precipitating out in the remainder of methanol that your rotovap didn’t remove.

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#16

I already pulled 10% of the weight in the initial winterizing.

It seems like there’s 200ml there, which would add up to about 55% of the volume of the initial extract. (Started with 386g)

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#17

Note* I also didn’t do the initial extraction, but their last few we’re a butane mix. I’ll ask about their intial solvent… maybe it’s something with a high BP (heptane?). But I can’t see why they’d have switched that.

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#18

The weight of the wax you pull off is greatly affected by the remainder of solvent in the wax. Even if it’s dry to the touch it will still contain a decent amount of solvent which will inflate the weight of the wax you pull off the filter.

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#19

I guess easiest thing to test if it’s a wax/fat would be to see if it dissolves in water?

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#20

Update, the yellow layer doesnt freeze at all and it’s freezer temps (-18c). Actually got more clear.

I’ll try boiling it tomorrow.

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