FASA: What Went Wrong?

[Poads]

I've done FASA before with ACRB. I thought I had it down pretty well. Last night I made my first attempt at a FASA extraction with MHRB, and I'm not pleased with my result. Here is everything I did.

1. Simmered MHRB in a water/vinegar mix for 2 hours

2. Separated the liquid from the sludge

3. Basified the liquid using lye

4. I used xylene as a solvent, and after the layers separated cleanly, I pulled the xylene layer

5. I put the xylene into a dish and I added FASA (mix of fumaric acid and acetone) a cloud formed, and I waited overnight. The cloud had cleared in the morning. So far so good?

6. I poured off the liquid. To my dismay, I was left with not what I recognize as DMT fumarate, but an orange/yellow goop that dissolves if I try to handle it.

I'm considering adding more FASA to the goop, but I really don't know what to do. This is not the result I expected at all.

 

[Poads]

Nobody really replied... so I'm gonna try to convert to freebase, then back to fumarate. Only problem, I have never done this before! Here's my plan.

I have dissolved the orange/yellow goo into water. It dissolved easily. I added a mix of water/soda ash. The solution got cloudy. I covered the container to prevent evaporation.

In 2 days (Thursday), I will filter using a coffee filter and (hopefully) get reasonably pure DMT freebase. I will dissolve the freebase into xylene and add FASA. Come Friday, I will (hopefully) have DMT Fumarate, which I will let dry first. I'm set on tripping on Friday.

Wish me luck!

Update: I did some thinking, and I probably don't need the xylene at all. Right now I have essentially a container with 3 things: water, soda ash, and the orange/yellow goop. I can see crystals (DMT Freebase?) at the bottom. Tomorrow I'll probably add pure acetone, which should dissolve the DMT Freebase. Then I'll add FASA, and that should get it to fumarate. Whether or not that will purify it, I have no idea.

I know this isn't the fastest forum, and I know patience goes a long way, but I really would appreciate it if someone with knowledge of FASA extractions could at least tell me if I'm on the right path. So far it has all been guess-work, and I don't know if what I'm doing is going to work.

Update 2: OR would I be better off adding heated naphtha to my goo/water/sodium carbonate mix, letting the DMT freebase dissolve into the naphtha, pulling the naphtha layer, freezing the naphtha, letting the DMT freeze precipitate, pulling the DMT freebase, dissolve into acetone, and add FASA??? What should I do????

Sorry for being such a noob about stuff like this. I'm annoyed that I'm even in this position... my FASA extractions with ACRB (besides my first one where I didn't know what I was doing) went off without a hitch... no converting to freebase, recrystallizing, or anything. I still have no clue what went wrong.

 

[expandaneum]

did you dry the acetone ?

 

[Poads]

did you dry the acetone ?

Considering that I don't know what that means, I don't think I dried the acetone. Care to explain?

 

[DreaMTripper]

Thats probably the problem the acetone cant have any water in it or the excess fumaric acid will also precipitate with the water hence the goo.
Freebasing wont be a problem but again if you do paste and pull the solvent must be anhydrous , have no water.
Search for 'drying acetone' many threads on it.

 

[Arcturus]

I think your xylene is faulty... but its only a feeling.

I would base the goop with sodium carbonate and pull with ipa / acetone, and see if anything crystallizes. As you mentioned.

 

[endlessness]

Add the FASA slowly, the slower the better.

If it doesn`t crystallize, I`d just mix the fumarate goo with sodium carbonate and bit of water to make a paste, let it dry completely, then pull again with acetone and add FASA as slow as possible (dropwise) to the acetone.

Good luck.

 

[Pickledpossum]

DELETED

 

[SomeYoungTraveler]

Could someone tell me an ideal volume of FASA at concisely how slow of a rate for say 400ml of xylene? I can't seem to find exact amounts or specific times as far as the FASA method goes and my fear is adding too much or adding it too fast :shock:
If anyone could give me a rough value for either/or, that'd be awesome!
And has anyone looked into the possibility of using fumaric acid in the acidification step on A. Confusa? I'm not sure if there would be a confliction between the pH modifying or not, but I think that would make incorporating the FASA approach into the tek alot simpler!:thumb_up:

 

[endlessness]

SomeYoungTraveler, Just add little by little. I dont think you have to worry, it's very forgiving. You can make, say, 100ml of FASA and add one ml at a time, till it stops cloudying. Let it stand for a day, add a bit more FASA and if it keeps cloudying, add more, if it doesnt anymore and stays clear, just let it stand for a couple of days just in case for everything to precip.

JimDandyCee, fumaric acid is most likely dry when you buy it already. A little of it dissolves, youre just not seeing it because you're adding too much. No problem, just mix well and then decant /filter away the acetone from excess fumaric acid

 

[concombres]

did you dry the acetone ?

Considering that I don't know what that means, I don't think I dried the acetone. Care to explain?

Get some epsom salts without dyes or fragrances. The ingredients should be 100% magnesium sulphate.
Crush & Dry it in the oven for a couple hours.
Add 20g per Liter of acetone, cap, shake, & let it settle for 24hours.
Pour some off thru a funnel with a cotton filter into a clean jar & use that for FASA.
The water content in the acetone is almost guaranteed to be what is causing you trouble.