I seem to have a problem with salting out

[Kneegrow]

I seem to have a problem salting out mesembrine and kratom alkaloids, this is what I do;

I first salt out the NP solvent 3 times with diluted HCL (approx ph 3-4), pouring out the alkaloid solution on a pyrex pan and then put it on a stove for medium/low heat until all water evaporates, I scrape up the salts but as soon as it's exposed to moist it turns into a sticky oil immediately! It also smells chlorine

Please guys help me out!

 

[Ayawasqero]

Call the chemist! Sorry...

 

[endlessness]

Im not sure of mesembrine and kratom, maybe they cant form stable solids for too long because the hcl salts are hygroscopic (thats what it sounds like)? Maybe you have to try with a different acid (fumarates for example) ?

By the way did you ever do an evap test on your hcl and see if by itself it evaps cleanly?

 

[Kneegrow]

Im not sure of mesembrine and kratom, maybe they cant form stable solids for too long because the hcl salts are hygroscopic (thats what it sounds like)? Maybe you have to try with a different acid (fumarates for example) ?

By the way did you ever do an evap test on your hcl and see if by itself it evaps cleanly?

No I didn't let it evap by itself but it was concentrated (30%) so it should be clean. So I should try changing acid and letting it evapping by itself without heat or it doesnt matter?
As I've understood fumaric acid is a powder? Won't that turn back into powder when evapped?

 

[endlessness]

Just because its concentrated doesnt necessarily mean its clean.

Yeah thats right fumaric acid is a powder, so ideally you add molar amounts of it to the acqueous solution so that there is no excess fumaric acid and all the fumaric acid added will be attached to your alkaloids once it evaps. Or you add excess fumaric acid and once its all evapped, you'll have some fumaric acid contamination, which you can clean up. But the problem is, I have no idea about mesembrine fumarate and its solubility in different solvents. With DMT you can clean by doing acetone/IPA washes, maybe it works for mesembrine too?

Or you try a different method of salting with fumaric acid, like the FASA method (dissolve alkaloid in acetone, add FASA, let alkaloids precipitate for some hours/days, decant/filter). Again I dont know if this would work specifically with these alkaloids you are playing with, could very well be but I dont know.

In any case you could only do those things with freebase alkaloids, because HCl is a strng acid so the chlorine ion will not be removed using weaker acids. So right now you would have to mix with sodium carbonate, make paste, dry, pull with solvent to get your freebase, and proceed from there to use another acid.

Im giving you a few ideas here to think about, personally im not interested in mesembrine and kratom and I never played around with them so I only speak theory here. Post back results

 

[dg]

easy solution, use less acid
fact, one pull should be plenty.

just google aqueous titration
basically, add only enough acid to reach the pKa of the alkaloid being extracted.

 

[Kneegrow]

I thought using too much acid wouldnt be an issue, but I guess I was wrong. I can't find the pKa of mesembrine, and the process with FASA seem very complicated so I guess I'll try with some concentrated acetic acid instead. Since I'm using a weaker acid, should I keep the pH at same level or increase it? Or should I keep using HCL just having higher pH?

 

[dg]

unreacted hcl will evap, so adding too much isn't really possible per se.
it will also pull impurities from solution if there is unreacted acid
using other acid is unlikely to solve your issue.

knowing the exact pKa isn't totally required

 

[Kneegrow]

I raised the ph a bit and changed acid to acetic acid, the results got better but still it isnt like a "regular" powder it keeps turnning to brownish solid crap as soon as it's touched, could it be due the way im letting it evap? I pour everything on a pyrex pan and put it on the stove for approx medium heat

 

[dg]

no, its likely not due to the way you evap.

ive had similar results using acetic acid,

there are further purification methods, they'll change based on what you are salting with, and what you have available...

here is what i've had success with

simple titration, and dual solvent crystalization - Preparation - Welcome to the DMT-Nexus