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got FASA precips, but i worry is only fumaric acid Options
 
caliwa
#1 Posted : 8/15/2011 3:33:34 PM

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I finally got a smokable ammount of yield, im using STB x pulling with xylene. I made warm pulls. I saturated some dried acetone with fumaric acid. i observed that must of the fumaric acid precipitated on the bottom of the acetone. I mixed again and add some drops to my xylene pull which was already on a wide glass jar. i waited till the cloud stoped, i added some more, waited again, and finally added some more, mixing the acetone each time since it apeared to me that if all the fumaric acid precipitated none would go to my xylene.

finally I decanted the xylene/FASA solution and observed that there was a lot of yellowish sediment on the botom of the jar. left all night in the window for all the solvents to evap. this morning I crasped the sediment and i got a good yellowish powder, my first thought was that I finally got some DMT. but thinking further, I think there may be a lot of fumaric acid in there, since my FASA solution was VERY saturated (i couldnt weight the fumaric acid so I eyeballed it).

could this be posible? that most of my sediment could be fumaric acid?

or

according to some chemical laws, if there sediment, its because fumaric acid added itself to dmt and all my sediment should be spice?
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endlessness
#2 Posted : 8/15/2011 4:15:18 PM

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caliwa wrote:
I saturated some dried acetone with fumaric acid. i observed that must of the fumaric acid precipitated on the bottom of the acetone. I mixed again and add some drops to my xylene pull


Saturating means no more fumaric acid can dissolve. It doesnt take much to saturate. So if when you saw that a lot did not dissolve and stayed on the bottom, it means the acetone is already saturated. What is on the bottom is excess fumaric acid. Then you mixed again, but did you let it stand again for it to decant away from excess or filter the FASA to remove excess acetone before adding to xylene?

If not, then there might be some excess fumaric acid in your end product together with your dmt fumarate.

caliwa wrote:


finally I decanted the xylene/FASA solution and observed that there was a lot of yellowish sediment on the botom of the jar. left all night in the window for all the solvents to evap. this morning I crasped the sediment and i got a good yellowish powder,


So you let evap/dry the decanted sediment, not the whole xylene+acetone, right?

In any case, the sediment should be your fumarates. Thats what happens when you mix FASA with xylene, the fumaric acid ions attach to the DMT molecule, and it makes it precipitate.

Your sediment is most likely spice, maybe with a bit of fumaric acid contamination. You could taste a tiny tiny bit of pure fumaric acid and compare with the dmt fumarate, it should taste different. In any case you can do a cold IPA or acetone wash which should dissolve fumaric acid but not your dmt fumarates (in any case dont throw the wash away just in case something goes wrong you can still save your alkaloids).

By the way, you do know you have to convert to freebase before smoking, yes? instructions are in BLAB tek in the wiki
 
The Day Tripper
#3 Posted : 8/15/2011 4:20:14 PM

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SWIM was under the impression that you could not precipitate extra fumaric acid with fasa, partly because any excess fumaric acid will stay soluble in the fasa/xylene mix. Its the fumarate salts that are insoluble in the acetone, so what you have should be salts and only salts.

Was your acetone completely dry?

If it is/was, swim recommends doing a wash of your salts in dry acetone. This will pull off any extra fumaric acid, and any fats/oils that may have made it into your acidic water.

Weighing it is the way to go swim says, he likes being able to know that if he put 300mg of fumaric acid in, and gets 1.3g of fumarates out, then that matches up with the ratios they should be at for dmt fumarate.

Finally, you mentioned a smokable yeild, i don't want to assume your ignorance, but you know that fumarates must be freebased before smoking, right? Smoking fumarates will tear up your lungs bigtime.

Good luck.
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caliwa
#4 Posted : 8/15/2011 5:05:30 PM

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Day tripper:

good thing to know that xylene/aceton solution solves fumaric acid, i dont think I saturated acetone that much for xylene not to solve what could have been extra added, and yes, I did the acetone dry tech. thanks for the weighing tip, i have to get a decent aparatus for that. thanks a lot dude!

endlessness:

You've got everything right my friend.I let evap the sediment, not the whole xylene/fasa solution. and yes, when adding FASA, i didnt let the fumaric excess to decant, since I thought acetone didnt solve fumaric acid, now I know what I see was the excess.
hey man thanks for always standing up for me in my questions, dont you think I dont notice that you are always behinf me on my extraction questions, i hope you feel how much I appreciate it.

I thank both for the fumaric conversion to freebase tip, the part of converting the fumarates to freebase sliped my mind, god thing I posted this.
I am with those man who own that particular kind of courage of the interior voyager.
 
caliwa
#5 Posted : 8/15/2011 6:35:17 PM

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one more question:

if I solve the fumarate sediment on hexane and then freeze precip, would it work? instead of the sodium carbonate precip?
I am with those man who own that particular kind of courage of the interior voyager.
 
endlessness
#6 Posted : 8/15/2011 7:44:57 PM

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No problem glad to be of help caliwa, this community helped me a lot too so all I can do is give some of that back Smile


and no, dmt fumarate does not dissolve in hexane, you need to freebase it for that to work.

If you wanted you could mix with sodium carbonate, add a bit of water and mix well to make a paste, let it dry completely and powder, then use hexane to pull the freebase

but imo its easier/nicer to have your product crystallize out of water, like its written in BLAB tek
 
caliwa
#7 Posted : 8/15/2011 9:26:25 PM

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yes i went through the BLAB tek, i will do it tonight like that. thanks!
I am with those man who own that particular kind of courage of the interior voyager.
 
 
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