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Question about salting out

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SyZyGyPSy

Tryptophilese Metaphysticus Anomalopteris III
So swim is trying to perfect his limonene tek so he can post a revised version... the only part that still feels kinda sloppy is the part where he salts out the alkaloids from the limo using vinegar.

So he asked me to ask you if anyone knows what the best way to go about this would be.

Say you've got some limonene with some magick alkaloids in it... say you're doing a pound of bark... and you're trying to salt those alks out into some gar in a sep funnel. How much gar would you use? How long would you let it set for? How many gar "pulls" or "saltings" should he do on the limo?

Any suggestions would be greatly appreciated. In the past swim has always used what he felt to be an excess of gar to make sure he got everything... but then he evaps all that gar and so he figures for the new tek he'd like to be able to tell people to use just enough to get it all. 'Cept he doesn't have a clue how much is "just enough."

Thoughts?

Thanks in advance,
SyZ
 
It is easy to find out, one just needs to know how much spice is in a single pull of limonene. This however is not easy to always know, so let's make some guesswork.

Let us say that one is pulling from 200g bark (A/B or STB, it doesn't matter) with some limonene, say 100ml. My guess would be that this limonene would hold roughly 1gram of spice.

So how much vinegar one would need to salt effectively this 1 gram of spice?

The answer is 0.318958511grams of pure acetic acid.

Or roughly in other words, 100 ml of a 0.32% acetic acid
Or 10ml of 3.2% acetic acid

But I guess for convenience and maximum results one would like to make 3 saltings out of this limonene with each salting 50ml of 0.6% acetic acid.

This amount on the 3 pulls would be enough to salt out almost 3g of spice, but it is always better to overshoot it a bit:wink:

Hope that helps!
 
so why not just evapping the limonene? I seem to remember that it left goeey residues, but couldnt one just redissolve in alcohol and enhance some herbs with it, or straight away rub some herbs on the goo? Ok, one wouldnt have the scales accurately but that is not the end of the world SWIM thinks

and if im not mistaken 69ron dude even talked about crystal spice but with some lemonene remains, but that it had wonderful taste and wasnt a goo.. unless I remember wrong, we must ask him
 
It seriously takes ages for limonene to evaporate. Good thing, it smells awesome, but why also waste it that way? The salting out technique allows it to be reused quite a few times.

I do not know how SyzyGyPSy's tek is planned, I presume he may attempt to basify the solution of dmt-acetate and pull with a small amount with limonene which, under evaporation will leave fairly pure spice and indeed a great taste of smoke.
 
Yeah limo takes forever to evap. Swim's old experiments were with a low grade of limo that left WAY too much residue for any kinda evap to be practical... even enhancing herbs, you wouldn't wanna smoke all that limo.
Swim has since found high purity limo that may leave less residue but he hasn't tried evapping it yet.
He salts out with gar then evaps the gar to reveal acetic salt goo. He redissolves that in a little hot distilled water (1oz per pound) and uses that solution as-is for oral administration at around 1ml per dose. Or he freebaseth it with sodium carbonate, pulls with iso, evaps the iso, revealing dimitrius goo and some sodium carbonate residue. Then he redissolves the goo in anhydrous isopropanol, leaving behind the sodium carbonate, and evaps the iso onto some herbage. Makes such a clean, powerful smoke if done correctly. It's a little more trouble than the other teks but the difference in quality is far worth it. There's such a drastic difference in effects... everyone who's tried it agrees, they never wanna smoke the petrochemical stuff again. Something you really gotta see for yourself.

Getting back on topic, another question...

Swim has some glacial acetic acid on the way. Should he dilute it first? OR just add it straight to the limo? Thoughts?

Thanks again for all your help!
 
Glacial acetic acid is basically 100% vinegar. As such, it is not of much use. It needs to be diluted to 5% or less to be used according to the intentions of the first poster.

Buuuuuuut.......it may still be possible to use it as it is. For instance, try dropping the glacial acetic acid in the limo containing spice and see what happens. It is very likely that acetic acid will make dmt-acetate and this will precipitate down.

One drop (from a dropper) of glacial acetic acid is around 20-30microliters. One drop of acetic acid can salt out 65-100 micrograms of spice. That is,

10 drops of glacial acetic acid can salt out 650-1000mg of spice.

It will be really nice to see this thing working, that would be seriously amazing. One can "test" the waters just by adding a few drops of glacial acetic acid in the limo pull and see what happens. It it gets cloudy, then presto! The clouds (=dmt-acetate) will very likely precipitate since they are not soluble in limonene.
 
Oh it definitely works. Swim has been using limo for the past couple years, and has sworn off working with petrochems altogether. His old write-up of the tek is already located in this section of the forum, and has been for some time. But it's real sloppy, he posted it back when he still didn't have it pefected just cuz he was so excited that it worked he wanted to share it with everyone right away. Now he's trying to work out all the kinks so he's got a cleaner, smoother write-up to go along with the cleaner, smoother product this tek produces.

He already knows from a post originated by burnt called "spice limonene update" that dropping pure glacial acetic acid into spiced up limo will indeed produce a cloudy precipitate that is indeed the dimitri being salted out.

Now he's just trying to figure out the optimal way to go about salting out.

You say it would be best to dilute it to 5%? Swim is curious as to why this is. Basically, it's a pain in the arse evapping all that water. The way swim's been doing it in the past is using vinegar, doing three saltings per limo pull as you mentioned above. By the time he's done he ends up with about a litre of gar that he evaps under a hair dryer. It's not too bad, he usually does it overnight and by the next day has his acetic salt goo ready for the next stage. But if he can cut that litre of liquid down to say 250ml, or even less, well obviously that would be better. So he's just trying to figure out ways to use as little volume of liquid as possible and still get all the spice. He's been intentionally using more gar than is probably necessary to get all the spice, but wants to optimize it before posting his revised write up if possible.

Another thought that he's had... what about testing the pH of the gar? Presumably the pH should go up as alkaloids go into the solution. If he adds more gar and the pH stays the same then presumably there's no more spice being pulled, right? Or would the pH change be too subtle to detect? Any thoughts on that?

Thanks again!
 
Why not just crash it out with hcl gas Twisted Evil
Click to expand...

Mainly just cuz Swim doesn't have any hcl gas.

However, just to report back... the glacial acetic acid works beautifully. It's nice to have that instant feedback so Swim knows when to quit doing pulls... just keep doing pulls until the addition of a few drops of acetic acid no longer clouds the limo significantly.

Swim adds drops, watches it could up, then adds just a little distilled water to catch it all. Lets it set overnight, separates, and evaps the aqueous layer, revealing his acetate salts. He then recycleth the limonene.

Thanks, Infindibulum, for all your help... turns out Swim was wasting way too much gar/acetic acid. Much appreciated.
 
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