Can you help with this problem with FAS-IPA?

[Luz]

Objective is DMT Fumarate.

1- I extracted MHRB to D Limo. (See picture of extraction column, a 3 ft column, 3 in diameter that is very effective and efficient.)
2- I saturated 99% IPA with Fumaric Acid (.5 g/100 ml) = FASI or FAS-IPA.
3- I dripped the FAS-IPA into the D limo getting a white cloud (apparently of very fine crystals) which eventually went to the bottom. (See pics, one clear, the other with one glass stirred up.) (Did not get the big white crystals predicted in the FASI info nor will the D Limo evap off any time soon.)

How do I get the D Fumarate out of this mixture? The mixture is D Limo with IPA with fumaric acid dissolved in it, with of course the white D Fumarate mini-crystals.

Obviously I can pour off the clear solution (D Limo + IPA + Fumaric acid) above, but my crystals are still in that same solution below. I am thinking washing with H20 is going to take with it the IPA and the Fumaric Acid (@ .63 g/100 ml) as well as the D Fumarate. The IPA will evaporate with the H20, then washing with Acetone or IPA will take off about .5 g fumaric per 100 ml and very little D-Fumarate. There seems to be no way to wash out the Fumaric of the acetone or the IPA, but these could be resaturated and used again as FASA o FAS-IPA?

Anyone know a better way? All considered, is it not more efficient to just use FASW? Although the D Fumarate is definitely much whiter here that with FASW.

All comments appreciated.

 

[Loveall]

How about filter (or decant) and wash that with dry acetone? After a quick dry you are done. Unless you went crazy with the FASI, there should not be too much fumaric acid left over. Also, the acetone rinses off residual limonene nicely.

I've never done FASW but I can imagine it takes a long time to evaporate and it will still have some persistent Limonene in it (see attachment there is a finite solubility of Limonene in water), so an acetone wash or a very long dry would still be needed to get rid of the lemon smell anyway.

How fast did you add the FASI? I've read that the slower one adds it, the bigger the crystals. Also, this allows to stop adding FASI at the end of the clouding which results in minimal excess fumaric acid. Crystals are affected by so many things (starting concentration, temperature, mechanical vibrations, etc) that you sort of never know exactly what you are going to get, but lower temps and slow growth seem to usually help.

Good luck.

 

[Luz]

Thank you for the file!

Acetone is soluble in D Limo so it would not wash or separate the Limo out of the residue, no?

For drying, I use a cardboard box with a hair dryer as shown in the pic. Works super well; will dry a cup of water in about 2 hours.

I went ahead and disolved the residue in water, separated out the D limo, dried off the H20 and IPA and washed with IPA to get out excess fumaric and limo and other impurities. The puriste crystals I have ever seen. My conclusion is that FASI is more work than FASW, but you can see what is going on at every step and the product is purer.

I started off putting it in slow, but did not give big crystals, only white smoke. I ended up just dumping all the FASI in.

By the way, I have a calculator for this process which shows how much FASI or FASW or FASA to use and how much to wash with to get out excess fumaric. I am attaching it and the foto.

 

[Loveall]

Acetone is soluble in D Limo so it would not wash or separate the Limo out of the residue, no?

I don't follow. If you want to wash the product to remove any excess fumaric acid + some difficult to evaporate Limonene, dry acetone does the job. This is because acetone dissolves what you don't want and won't dissolve the product. Right? Dry IPA also works in the same way (but it will remove excess fumaric acid better).

For drying, I use a cardboard box with a hair dryer as shown in the pic. Works super well; will dry a cup of water in about 2 hours.

That's a cool setup You probably know this already, but be mindful when evaporating a lot of alcohol when a heat element is involved. Should not be an issue here, just something to keep in mind, especially in an enclosed area.

I started off putting it in slow, but did not give big crystals, only white smoke. I ended up just dumping all the FASI in.

As I understand it, you need to let that initial cloud settle, give it a chance to coalesce and form something like "seed" crystals. Then make it cloudy again and give that sometime to attach to the "seeds". Keep on repeating that. Takes patience. Give it a shot if you are up for it and see if you notice a difference. By the way, I could be wrong here - I hope I don't waste your time.

By the way, I have a calculator for this process which shows how much FASI or FASW or FASA to use and how much to wash with to get out excess fumaric. I am attaching it and the foto.

I can't open it on my phone but I'll say this: :thumb_up: