Accessory alkaloid sulfate solubility?

[Elrik]

Spoiler question: Does sulfate allow easy separation of mescaline from other stuff?

So I have a jar full of this trichocereus alkaloid that is kind of speedy for mescaline and only half as visual as my best mescaline. I've been using it in experiments because, while I like it, I'll more easily accept loosing some here and there in experiments. One possible project on my list is using it to trial chromatography guided separation by recrystallization in different solvent systems. But I think I stumbled on to something.
To date I've always worked with the hydrochlorides of cactus alkaloids. In trying my luck with sulfate I dissolved a gram in 15ml near boiling water, filtered it, crystals formed as it cooled to room temperature, I then maintained it in an ice bath for most of a day before vacuum filtering. I got back ~40% of the input in crystals.
Mescaline sulfate is listed as almost insoluble in ice water. Did I just remove the diluting alkaloid that made this batch speedy and less visual?
Has anyone intentionally cleaned up alkaloid in this way?
Did I just save a month messing with methanol, ethanol, propanol, butanol, acetone, and other things? :lol:

I'd do a test crystallization with my best mescaline but I ate it all.
Funny how that always happens

 

[antichode]

Once I’ve reduced my aqueous phase (I target about 20ml water per gram of mescaline). I do an initial quick crystallisation dumping in two times the volume of acetone. This always causes rapid precipitation).

From there I proceed to a second recrystallisation directly from water doing much like what you have done although here I target 10ml per gram. Starting at room temperature then into the fridge. Then decant the water underneath the crystal and wash any residual water away with acetone. This way takes a lot of crap out of your end result as almost everything is soluble in water other than mescaline and I find I usually lose up to 20% of what crashed out in the first step. Some of this is certainly mescaline so You do sacrifice some yield but you gain purity, Sulfate achieve this so easily. I’m not sure what makes up that remaining 20% but it certainly feels a bit different to mescaline. Although this could just be my own bias at seeing it separately. It feels Speedy as you descriBe but then I find all mescaline EXTREMELY stimulating. 400mg will keep me up for at least 24hrs

 

[Orion]

I'd love to know too. Anything definitive and simple when it comes to cleaning up mesc would be nice. There are lots of methods but the results vary too wildly to risk losing the small amounts one usually has. Bioassay requires commitment and time and a fair bit of experience.

I'd move to sulphates if all it took was cold water. Or fumarates if we could prove whether or not crashing with FASA or FASI creates accessory salts. I've heard completely opposite opinions on it from fairly experienced people.

 

[antichode]

Sulfate crashes readily from cold water. Heck you don’t even need acetone to get very clean crystals, that picture i posted here Mescaline base partition ratios, do we need them? - Preparation - Welcome to the DMT-Nexus is while the water was at 30deg C. Before I put it in the fridge!

 

[Elrik]

It's good to have some confirmation on this. I knew this batch was just packed with accessory alks, but I was still surprised to loose 60%. It fits on the level of visuals, though.
Assuming my non-crashed alkaloid proves to [predominantly] not be mescaline than if nothing else I'll save the fraction to mix with caffeine. 60mg of the parent alkaloid•HCl taken with a strong cup of coffee is my secret weapon for 8 hours of stimulation and appetite suppression to get work done. I have invented the mescaline diet
Perhaps some other use can be found, as well. Like ayahuasca admixture. I've gone as deep as 750mg speedy alkaloid•HCl [= 938mg sulfate] in combination with harmine, twice, and nothing bad happened. Unless you count tripping my freaking Brains out :lol:

It'll help resolve some of these questions if a good chromatographic eluent for mescaline vs. accessories is worked out. If I can see different spots with different Rf values it will make evaluation of the product less subjective.

Spoiler

Solvents I have available to use in an eluent include methanol, ethanol, isopropanol, butanol, acetone, butanone, ethyl acetate, chloroform, toluene, xylene, isoöctane, turpentine, limonene, and 10% ammonia (aq)

Okay, so I'm on the right track, I should just isolate the byproduct to test separately.
Right on :thumb_up:

 

[antichode]

I've gone as deep as 750mg speedy alkaloid•HCl [= 938mg sulfate] in combination with harmine, twice, and nothing bad happened. Unless you count tripping my freaking Brains out :lol::

:surprised That would do it alright! Last time I had 400mg. Took it at 9am hoping to imbibe then sleep that night but nope! All visual effects were gone after 12 hours or so but mescaline leaves me feeling wired for hours and hours afterwards. Didn’t sleep a wink untill 9am the next morning. Alcohol or Zoloft work but that’s such a bummer way to end the greatest drug in the world!

 

[Loveall]

Once I’ve reduced my aqueous phase (I target about 20ml water per gram of mescaline). I do an initial quick crystallisation dumping in two times the volume of acetone. This always causes rapid precipitation).

From there I proceed to a second recrystallisation directly from water doing much like what you have done although here I target 10ml per gram. Starting at room temperature then into the fridge. Then decant the water underneath the crystal and wash any residual water away with acetone. This way takes a lot of crap out of your end result as almost everything is soluble in water other than mescaline and I find I usually lose up to 20% of what crashed out in the first step. Some of this is certainly mescaline so You do sacrifice some yield but you gain purity, Sulfate achieve this so easily. I’m not sure what makes up that remaining 20% but it certainly feels a bit different to mescaline. Although this could just be my own bias at seeing it separately. It feels Speedy as you descriBe but then I find all mescaline EXTREMELY stimulating. 400mg will keep me up for at least 24hrs

I'm trying to find an example of the solubility of mescaline sulfate in water at fridge temperature.

So based on the info above, <200mg dissolve in 10ml of water (<2% solubility). Maybe half of that is mescaline (since the comment is "some of this is certainly mescaline"?), that would be guestimating the solubility of 1% ~ 0.02M (using 556g as the molecular weight of mescaline sulfate dihydrate).

Has anyone measured examples of mescaline sulfate solubility in cold water?