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DMT fumarate conversion comparison (pics)

Migrated topic.
I'm trying to understand why Vinegar evaporates produce a very hard-to-handle runny dark goo freebase; compared to when one takes fumerates and does the sodium carbonate conversion to freebase? I believe this can be done with 99% IPA as well. Maybe I am missing that the full range is not completely present in the original fumerate step, as compared to salting out with vinegar.
IS this the reason?

Thanks for helping me understand this. I will try to look over the threads to find the answer.

It could be that I was under the impression that FASI yielded a full range fumerate product, but this may not be the case.
 
One of the reasons could be more n-oxide present in acetates than in fumarates from FASI for example. In this very thread if you read further back I had a discussion with infundibulum about n-oxide. He affirms it could be possible to have n-oxide fumarate, though I wonder how easily it is formed, in, for example FASI, maybe only small amounts? While chemically it will definitely be in the evapped vinegar acetate if it was there in the first place. So I think thats one main reason.
 
My mind was slow initially; I just grasped the beauty of the water precipitation clean up. Excellent!
Maybe some loss is worth it to keep it clean/green.
If the yield is the same as IPA clean up, and the product cleaner and purer, then no doubt this seems like the best system for pure spice yet.

Endless, I know you like to do some things by eye, and I'm sure you've earned your right with your experience

Would you please consider suggesting a basic formula, i.e., a ratio of water and then how much saturated Sodium Carbonate solution to add to the water.

If per chance there was any residue present in the drying water, then keeping the Sodium Carbonate water to a minimum would be helpful toward this end.
And, is there a chance that keeping the water volume to a minimum would be of any benefit toward minimizing loss during process?

I would have to imagine that if this was done with a gallon of water with one gram fumarate spice, then the loss would have to be more?

Judging by your pictures -- and those look like Pint drinking glasses, you dissolved 1 gram spice in about 4 oz hot water.
Then you added 1-2 oz saturated sodium carbonate solution.
And then you waited a couple days but did not refrigerate because this would be unnecessary.
 
Infundibulum said:
Whoa, nice to see that people try this thing again!

Endlessness, please note that the water precipitates from the basic solution will have traces of sodium fumarate as well as sodium carbonate that are inevitable on the watery dmt crystals. SWIM had to wait for the dmt to dry, then dissolve it in acetone to get rid of the contaminating salts.
Click to expand...
And so filtering out the acetone through coffee filter to keep the fumaric and carbonate traces in the filter, and recollecting the crystal in hte evaporation dish ?
 
rOm said:
Infundibulum said:
Whoa, nice to see that people try this thing again!

Endlessness, please note that the water precipitates from the basic solution will have traces of sodium fumarate as well as sodium carbonate that are inevitable on the watery dmt crystals. SWIM had to wait for the dmt to dry, then dissolve it in acetone to get rid of the contaminating salts.
Click to expand...
And so filtering out the acetone through coffee filter to keep the fumaric and carbonate traces in the filter, and recollecting the crystal in hte evaporation dish ?
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Yes, even though when SWIM was working on this method he was a bit lazy and he was not decanting off all the water and he was not filtering properly etc. For these reasons his precipitated freebases had a fair amount of residual water and thus sodium fumarate and sodium carbonate. But if one filters properly as endlessness did then there should be no significant amount of neither sodium fumarate nor sodium carbonate.

The latter is important to those who want to keep on the food-safe path for as much as possible and do not want to mess with potentially non-food safe acetone. If one has enough acetone then he may as well go for the paste method instead of the water precipitation.
 
So he has to use ACE to clean his crystals from impurities ?

He will loose the food-safe quality of his initial product or did I understood wrong ?
 
Sounds to me like Vacuum Filtration with the basified water precipitation is the way to go.
IF the minimum amount of saturated Sodium Carbonate solution is used -- which I am trying to figure out -- then contamination should be at a minimum.
Unless one really enjoys working with acetone.
Besides, look at those pictures, that is amazing, pure spice with ALL food grade processes!
 
Plumsmoth, I don't enjoy a lot working with acetone, just when there is no way around (looking at the solvents available).
When I see these picture, I think the same as you, both the SWIM speak about use limteks for the reasons of staying food safe whenver it's possible.
What is vaccum filtration ? Do you mean sucking out the basified water to leave crystals behind ? If so, why was it discussed here the residue could be wash (actually maybe in traces amount the bases and acid are not toxic to vape...
 
I think acetone is a very nice solvent to work with actually, but I get it food/USP grade.. I dont know about hardware store acetone, thats always very uncertain, I would be wary of trusting that....

In any case if you just read the thread again you'll see that acetone is not really necessary to clean up. As infundibulum said, when he tried this method he wasnt so careful in his separation of the crystals from the water it crystalized in, so he had some impurities (sodium carbonate and sodium fumarate).

Nevertheless, the amount of these impurities present in the final product is negligible if you just filter it till dry. Vacuum is useful but not necessary. r0m, if you dont understand the process of vacuum filtration I suggest you look it up, its very simple.

and yeah, in any case, trace amounts of sodium fumarate and sodium carbonate are not really gonna hurt you :)
 
endlessness said:
Note: The water precipitation does not work with DMT acetate dissolved in water (neither with filtered mimosa brew), as tested by myself and others, probably for the reasons explained by Infundibulum in another thread, so it has to be redissolved dmt fumarate
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I tried this method with acetic acetic acid. It worked fine. First it turned milky white, and over the period of 1-2 days it formed crystals and lumps on the bottom of the glass. The procedure was done after extracting dmt from limonene, by adding acetic acid. Lye was then added to the resulting liquid, giving dmt freebase.
 
really?! very interesting, I tried it twice and it didnt work, once nothing precipitated, the second time it was a small goo on the bottom.. It was with vinegar though, not glacial acetic acid, maybe that makes a difference.

What was the yield like, in terms of weight and looks?

by the way, this was added to the wiki:

Fumarates to Freebase Conversion TEK - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me
 
endlessness said:
really?! very interesting, I tried it twice and it didnt work, once nothing precipitated, the second time it was a small goo on the bottom.. It was with vinegar though, not glacial acetic acid, maybe that makes a difference.

What was the yield like, in terms of weight and looks?

by the way, this was added to the wiki:

Fumarates to Freebase Conversion TEK - DMT-Nexus Wiki
Click to expand...
Maybe the sodium hydroxide made the difference here? Endlessness, did you try the basification with NaOH or sodium carbonate?
 
hmmmmm.. the sodium carbonate basing of the vinegar pull was the one with no yield, while the one with small amount of goo, I had used NaOH... though to be honest its possible in this second one that I had first tried to precipitate with sodium carb and then added NaOH later, I dont remember much, so that also might have made it screw up.

So would be interesting to make tests with:

1- Vinegar salting vs dilute glacial acetic acid salting.
2- Sodium carb precipitation vs NaOH precipitation
 
I used 35% acetic acid. I don't know what the yield was, but I got ~600mg freebase spice from some brews that has been standing for years. The results was nice and fluffy, slightly yellowish with a smell of limonene.

Here is a picture before it has dried.
 

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I just started this last night.

I only used 2.5 oz of water to dissolve 1.91 grams of DmtFum. And then added the carbonate solution slowly which was only around an oz of liquid all together.
I have this mixture sitting in a pyrex measuring cup in the fridge and I'm worried that the 3oz of liquid in there is too little for whatever reason.
I never have much confidence in any new procedures even though I essentially have a 100% success rate with everything I've tried.
12 hours later and I do see some particulate settling on the bottom but nothing yet stuck to the glass.

When I dissolved the DmtFum there was a bit of particulate that wouldn't dissolve. Just a few off color specs of stuff that definitely came from the Dmtfum. I was going to decant the Dfum solution but somehow forgot. Is there any chance that this foreign material, little as it may be, could effect the outcome?
 
there is no reason I can think of why 'too little' water would make it a problem. Dont be affraid of things just because. If all is done right, it will work fine, and if something doesnt go as expected, just dont throw it away an it can always be saved. 12 hours is not enough, wait 3-5 days, the more the better.

As for the particulate that didnt dissolve, did you use warm water? Can you show some picture? maybe it was just a bit of dense dmt crystals.. you should give it enough time and stir to dissolve all.. Maybe,though, its some dust or whatever that came in and it wont dissolve. .This you could just decant or filter to remove it. Dont throw it away just in case there is some actives there, it can be recovered (though I guess its just dust or something). But if you dont want to do anything there, just leave it and it will be small contaminant in your final product, maybe you can even remove it manually once your freebase dmt has formed

You are probably doing just fine. good luck!
 
endlessness said:
there is no reason I can think of why 'too little' water would make it a problem. Dont be affraid of things just because. If all is done right, it will work fine, and if something doesnt go as expected, just dont throw it away an it can always be saved. 12 hours is not enough, wait 3-5 days, the more the better.

As for the particulate that didnt dissolve, did you use warm water? Can you show some picture? maybe it was just a bit of dense dmt crystals.. you should give it enough time and stir to dissolve all.. Maybe,though, its some dust or whatever that came in and it wont dissolve. .This you could just decant or filter to remove it. Dont throw it away just in case there is some actives there, it can be recovered (though I guess its just dust or something). But if you dont want to do anything there, just leave it and it will be small contaminant in your final product, maybe you can even remove it manually once your freebase dmt has formed

You are probably doing just fine. good luck!
Click to expand...


Thank you for that encouragement. I'm just a worrier. Something I'm constantly trying to correct.

I think that which didn't dissolve, which was given ample stirring, time and proper water temp, was just some dust or something else that, for the most part, is insignificant. Of the 1.91g of DmtFum it was probably .001% that didn't dissolve.

Thanks also for all your work and documentation.
 
I think acetone is a very nice solvent to work with actually, but I get it food/USP grade.. I dont know about hardware store acetone, thats always very uncertain, I would be wary of trusting that....
Click to expand...

I agree. Acetone is easily one of the safer solvents people can use. Check out these LD50 numbers.

RTECS#:
CAS# 67-64-1: AL3150000
LD50/LC50:
CAS# 67-64-1:
Dermal, guinea pig: LD50 = >9400 uL/kg;
Draize test, rabbit, eye: 20 mg Severe;
Draize test, rabbit, eye: 20 mg/24H Moderate;
Draize test, rabbit, eye: 10 uL Mild;
Draize test, rabbit, skin: 500 mg/24H Mild;
Inhalation, mouse: LC50 = 44 gm/m3/4H;
Inhalation, rat: LC50 = 50100 mg/m3/8H;
Oral, mouse: LD50 = 3 gm/kg;
Oral, rabbit: LD50 = 5340 mg/kg;
Oral, rat: LD50 = 5800 mg/kg;

The source for that is here: http://fscimage.fishersci.com/msds/00140.htm

I also agree that hardware bought Acetone in a metal can likely has some sort of anti rust additive in it....not positive here...and probably not that big of a deal.

I still say that from the home hobbiest perspective re-crystallization is going to be the purest form people can obtain. Vacume dry if you want, but I'd vacume dry after a recrystallization step. I say this NOT having done every tech out there...nor do I even plan to. I may try a straight to base route if I do this again in the future, but maybe not. I like the control an A/B affords me.

BTW one can find nice hand held vacumme pumps that can be connected to Erlynmeyer flasks that work quite well for separating crystals from solvent in a filtration step...this however is NOT the same as vaccume drying. For that you will need an electric vacumme pump...and a few other pieces of lab equipment to do it effectively...a rotovap would be ideal.
 
36 hours in and its looking good but I'm noticing that the crystals don't seem to be sticking to the sides of the jar as they do in the pictures. Instead they are just floating on the top of the solution.

I wish I had a camera.

EDIT 1: I've now pulled it and it's drying. It still has a tan color to it and I'm wondering if it's possible that it's somehow still fumarate. Once dry I'll weigh it to see what was lost and I've put the left over solution back in the fridge to see what comes of it.
EDIT 2:I mean...if it was still a fumarate it wouldn't have precipitated out of the SodiumCarb/water solution right?

EDIT 3: Well it's not soluble in water whatsoever so it surely isn't fumarate. I guess my freebase just didn't turn out to be white is all.

EDIT 4: Mine came out to look more like the acetone tek but after vaping it I'm happy to see it burns away clean.
 
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