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Fumaric acid crystals

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ms_manic_minxx

ms_manic_minxx

Esteemed member
OG Pioneer
I'm making this post in light of something Jorkest mentioned in his Phlaris thread: FASW works well for MHRB + me, but, I can never figure out how much yield is actually present until freebasing. I always have tons of excess fumaric acid, even after washing (with distilled water), and it doesn't seem to fully get lost until the freebase step.

After freebasing, yields are still nothing to complain about, around 1%, but it intrigues me greatly to hear a more detailed explanation of what this phenomenon is. There is nothing air-tight or covered in my process.

Thank you!

Love,
-She Who Slowly Grows In Understanding :)
 
If you know about how much fumaric acid you had in the FASW, subtracting that weight from the first evap's yield will give the amount of freebase present. If you know this exactly, and still seem to be losing product in the freebasing procedure, then something's being lost to the conversion methods. In such a case, SWIM would suggest giving his nontoxic conversion a try, as it can convert and make ready the full yield in a clean and expedient manner (no toxics or evap time).
 
This is a major problem with the initial fumarate salts. The only way to remove it is to do water recrystalizations. There is a tech and post on it SWIM made a while back. Dissolve everything in a small amount of hot water. Let cool at room temperature and open to the air (to evaporate) for a day or so....or so.... before all the water evaps (when there is maybe 1/5 of the original volume) collect the crystals. They should be "large" and transparent and look like rock candy.

Don't throw the water out but evap and perform again for a second crop of crystals.

This works amazing but requires some patients. If one is gonna convert to FB anyway then there is no need. People weigh their FASA and think they hit the jackpot and then FB and think they screwed up. Dn't worry One is not lossing product as there can be over 50% fumaric acid present in the FASA salt.
 
bufoman said:
This is a major problem with the initial fumarate salts. The only way to remove it is to do water recrystalizations. There is a tech and post on it SWIM made a while back. Dissolve everything in a small amount of hot water. Let cool at room temperature and open to the air (to evaporate) for a day or so....or so.... before all the water evaps (when there is maybe 1/5 of the original volume) collect the crystals. They should be "large" and transparent and look like rock candy.

Don't throw the water out but evap and perform again for a second crop of crystals.

This works amazing but requires some patients. If one is gonna convert to FB anyway then there is no need. People weigh their FASA and think they hit the jackpot and then FB and think they screwed up. Dn't worry One is not lossing product as there can be over 50% fumaric acid present in the FASA salt.
Click to expand...

Heh...I was just about to post it. Here it is: ........*Hmm, it's a little different than what you posted here ^^.

"Bufoman's Method of Removing Excess Fumaric Acid:

To separate the desirables from the fumaric acid one simply adds 12mL H2O per gram of material. (the DMT fumarate is soluble in the water while the fumaric acid is not).

The aqueous (now yellow) solution is carefully decanted into a clean beaker or drying surface.

The water is reduced by 1/2 with a hair drier and then allow to sit open to the air and slowly evaporate.

Within a day (at most) large transparent crystals will begin to precipitate out one can collect these. (If one does not care about ascetics the solution can just be rapidly evaporate with a hair drier or on the oven and the crystals utilized right away. However SWIM recommends the crystallization.)

The remaining solution is then reduced again with a hair drier and allowed to sit as before. Once it has fully evaporated the crystals can be collected.

One now has highly pure DMT fumarate. The crystals are very nice to look at. One can attempt to wash the fumaric acid crystals again with an additional 10mL of H2O to see if any crystals are obtained however due to its solubility most of the DMT fumarate will collect during the first attempt."
 
ms_manic_minxx said:
I always have tons of excess fumaric acid, even after washing (with distilled water), and it doesn't seem to fully get lost until the freebase step.
Click to expand...

Based on this, SWIM thought she had already performed water purification. SWIM hopes that minxx wasn't trying to wash off fumaric acid with water.


With the last water purification/rextal that SWIM did, he reduced the water volume a bit much and left it in the fridge and in room temp for a while using a small custard dish. He ended up with a hard disk of deep red fumarates (full-range from jurema) which broke into shards and bottled. Most of the time, he just does a hasty rextal by evaping completely on a wide shallow dish, moistening the surface lightly before scraping (if this isn't done, it is very difficult to scrape up, and you'll make a mess), scrape the wet fumarates into a pile and pop it back in the dehydrator; if SWIM does this right, he gets rocks, otherwise, it turns out a bit sandy. Sometimes, if there's enough fumarate concentrated in a small area and is hot enough, it will form a goo, and this goo can be worked around to solidify into very dense and solid rocks.

Freezing the mixture of limonene and FASW to induce separation of the limonene from the aqueous solution (so it can be decanted without aid of a separatory device) also precipitates out excess fumaric acid prior to freezing solid (perhaps not all of it, but most...still needs more testing). Freezing is a great, multi-purpose preliminary step when dealing with FASW, in SWIM's experience
 
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