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Fumaric acid solution is super yellow

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21stCenturyAlchemist

Rising Star
To start:

Followed Jorkest's tek to the T. Ended up with highly orange d-limo (first oddity). After salting, ended up with highly yellowed fumaric acid solution. D-limo is still very much yellow-orange (looks like it toned down a little through the salting process).

Evaporated to a brown goop which was to be expected, and then freebased using amor-fati's tek. the result was super-harsh, super-basic smoke. As as result, dried clay-like stuff was re-imersed in saturated sodium carbonate with the yellowed dmt-fumarate acid solution.

The solution was shaken in a vessel and refridgerated, following Endlessness's post on fridge preciptation. Brown chunks with clear crystals coming out of them precipated out. Half was collected to test out. In the process of testing, the chunks and crystals all melted into a brown phlegm-like goop which smelled heavily of D-limo (????). Took a portion of that goop with a knife-tip and lit it to see if there was any spice within it. Smelled somewhat like spice, so it turns out there is spice still in the goop.

Took the goop which had then bled into paper filter and washed it with acetone onto a dish. Nothing dried out of it. All that was left of it was a slippery film on the bottom.

Took the other half of the brown goop that was still in the fridge, and left it in a jar to melt down. It melted into a whitish water solution with yellow oil drops suspended. It was put onto a plate to evaporate. It evapped into a white film which was scraped and then put onto a glass funnel with a cotton filter. Then acetone was dripped through the white chunks through the filter onto a dish. The acetone is evapping slowly with some whiteness in it... Swim assumes that's the potential spice hidden away in all that goop/sludge/gunk/films/whathaveyou! The yield after all of that is extremely marginal. Swim feels like that there is still spice in the fridge jar that has not precipitated. Swim also questions the fact that the solution is still heavily yellowed.

Now the question is... The D-limo solution was salted some more with heavily saturated FASW. The result was again a super-yellowed water seperation on the bottom. This saturated water was filtered through a cotton ball, and the current question is.. Why are these solutions so very deep yellow? Swim has browsed the forums to find to no avail anything on this oddity.

Should swim evaporate that water like usual, and instead of following amor fati's freebase technique, stick with Jorkest's????
 
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So all the acetone evaporated and still left a puddle of goop stuck to the dish... Could this be a problem with some impurities in the D-limo? and if so, perhaps I should try doing a naptha pull with the water so that the impurities in the D-limo don't get saturated into the solution?
 
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The naptha, after being mixed with a saturated solution of [supposed] dmt-fumarate and NaCO3 water, turned yellow. It was subsequently placed into the freezer for a day. What precipated out of it was yellow grains which smelled somewhat like dmt, but left yellow stains on the coffee filter.

A recrystalization of the grains showed absolutely nothing but a clear film of goopy stuff. The precipitated mass of the grains looked like less than 50mg.

Swim feels like there is spice somewhere in all of this mess as there keeps to repeated whiffs of it, yet, cannot materialize a single pure crystal, using all of the above methods...

Swim also wonders if it's just too hot where swim is and that his actual crystals are melting into goop (it did get to 114 degrees two days ago..)... But that does not explain the d-limo smell in the supposed 'pure' final product....

Any help on this would be greatly appreciated.
 
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Wow what a mess, its really hard to get a sense of what you did there....

I guess easiest to do would be to take whatever you have where your alkaloids should be (the goo, the filter that absorbed some melted dmt, etc), redissolve in small amounts of acidified water, then re-base the water, and re-extract with simple solvent like naphtha, freeze, and retrieve crystals with the upside down trick as written in faq question 4.17

Tomorrow I can try to decypher a bit more your words and give more in depth tips but for now I would say that what I just said is your safest bet to get some dmt there..
 
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SO far Swim has followed Lazyman's STB tek and never ended up with anything more than a basic mess of bark sludge. Swim has followed Vovin's tek and came out with beautiful crystals, but did not like the toxic solvents. This encouraged swim to do more research and came across Jorkest and Amor Fati's tek, which seemed more holistic. After the first attempt with no idea as to what could have went wrong, swim is disheartened that swim is resorting to the toxic solvents JUST to get SOMETHING out of all that hard work..

Keep in mind the average temperature out here (without A/C) is in the upper 90s to the hundreds.. So Swim is starting to feel like swim's impure dmt is melting due to the impurities giving the dmt a lower melting point... But then swim also wonders how anything but pure or oxidized dmt would still be bound to the molecule after dissolving into naptha.

Argh.
 
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a few more thoughts:

it sometimes happens that limo pulls a lot of impurities, and salting with FASW ends with a quite crude product. If the product has too many impurities, it could mess up the fridge crystallization. You can def still get crystals from limonene based teks, maybe the only thing you would need to do, which would be a little extra trouble, would be to get your evapped FASW, redissolve in a little bit of warm water, re-base, and re-extract with limonene, re-salt, and then do the water crystallization. This second time around, you will already have a much purer product.

Also, notice that limonene often leaves residues in the FASW, even if you separate it really well (and it only takes a tiny drop of limo to make your product smell a lot of it). To get rid of limo traces, do cold (and dry) acetone washes on your dry fumarates.. then do the conversion thing.
 
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Thanks, swim will try that too...

Out of curiosity, swim looked up the MSDS of swim's particular d-limo.. and it is in fact 100% citrus terpenes and nothing more.

So to clarify:

Swim has a solution of FASW+NaCO3 water with potential alkaloids.

Swim also has super yellowed d-limo that just today swim added more FASW to the d-limo.. And again, the FASW is super-yellow.

So.....

Should swim take his FASW+NaCO3 and evap that to a sludge/clay consistency? And then RE-DO the entire tek (basically) from beginning to end, but instead of doing it to the root bark+lye water, do it to the chunked up, extracted sludge instead?

And then do water crystallization...?

Ok, Swim was afraid of having to use acetone, but Swim supposes that is much better than using naptha.. Somewhere along the lines there's gotta be a light at the end of this dark tunnel.

One other question is, and I'm not sure if you would know this endlessness, but would the impurities that the d-limo pulled make it all the way into the naptha wash??? Is acetone the only true way to get rid of the limo????
 
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hmm the solution with FASW + NaCO3, didnt something precipitate out of that?

Keep the FASW+NaCO3 water for the moment, but your alkaloids should have been mixed with whatever precipitated, even if it seemed very impure.. So get whatever precipitated + the other goop you said that stained the filter and that you tried to re-x, and redissolve that in warm vinegar+water solution.

and yeah, re-do tek with whatever product you have at the moment (instead of with mimosa).. Think of it like, the first run, you already cleaned it a bit from plant material, now you have a cleaner starting product that will get even cleaner.

Acetone is present in small amounts in fruits, for example, we're exposed to it on a regular basis. Plus it evaporates really fast and cleanly (make sure you get a clean-evapping acetone that has no weird stuff added).

Im not sure what naphtha wash you are talking about but if you're using naphtha, I think it beats the point of using limonene in the first place...

Running the FASW water through funnel with cotton plug helps getting rid of some limonene. Separatory funnel would also make for a cleaner separation.

But yeah the most effective way to get rid of limo traces would be washing the dried salts with a solvent that doesnt dissolve the fumarates, such as acetone (and as I said, acetone is "natural " enough).

In the end though, a little limo traces wont hurt you, it just smells of oranges ;)

BTW, what is your smoking method?
 
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Current smoking method is usually an herb screen on a glass chillum.

Well the first time acetone was used, it ended up in a goop.

So my question to you, Endlessness, is how did you end up with pure white crystals from fridge preciptation without all the orange goop surrounding them? Did you clean up your FASW solution a bunch of times before mixing with the bass solution? And if so, how did you do that?
 
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Sounds like your smoking method might be very harsh. I would try in the very least a bong with ash sandwhich and going very easy with lighter, but ideally spending on GVG and a torch lighter (its sooo worth it! )

What do you mean with "first time acetone was used, it ended up in a goop"? When was it used in the process? what was the starting product, what did you do, etc?

As for pure white crystals, yeah I did have it without orange goop. My fumarates were reasonably clean to begin with. But I also did the exact same process and the FASW came out some red goo, which I tried all sorts of different ways to clean, like acetone and IPA washes and also recrystallizations and so on. I think if it is sooo dirty when you evap the FASW, the most effective to clean up is doing a re-a/b (in other words redissolving and re-extracting). It might seem silly to have to repeat but thats how it is with chemistry sometimes, you're purifying the product. Take it like meditation, alchemy :D
 
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Took the goop which had then bled into paper filter and washed it with acetone onto a dish. Nothing dried out of it. All that was left of it was a slippery film on the bottom.

Took the other half of the brown goop that was still in the fridge, and left it in a jar to melt down. It melted into a whitish water solution with yellow oil drops suspended. It was put onto a plate to evaporate. It evapped into a white film which was scraped and then put onto a glass funnel with a cotton filter. Then acetone was dripped through the white chunks through the filter onto a dish. The acetone is evapping slowly with some whiteness in it...
Click to expand...

and it evapped into yet another white film...

so it makes me wonder what repeated evaps would do if it just ends up as films of whiteness..

Ok, so swim ended up with extremely impure and harsh brownish-white clumps (which probably would have been excellent as pharmahuasca) as per amor fati's tek. It seemed like "Yay! Results."

In the attempt to smoke it, it tasted heavily like base (like smoking too much NaCO3).

This prompted swim to endure purifying this end product to crystallization... What swim did was re-liquified the gunky product in FASW.. and then re-basified the solution, and THAT is what ended up going into the fridge for precipitation.

And THAT is what ended up precipitating orange clumps surrounding beautifully clear crystals that melted in the heat of the day to a depressing, oily puddle of sadness.

And that is when the acetone comes into play.
 
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Ok so, you used acetone to dissolve the impure freebase and to re-evaporate. For sure it didnt clean up because acetone dissolves dmt freebase as well as impurities. The only thing you would be cleaning of, which wouldnt dissolve in acetone, would be sodium carbonate, for example. When I talked before about acetone wash, I said acetone wash on the fumarates, which would not dissolve the fumarates but would dissolve impurities (like limonene). If you want to clean what you have, and try to get pure crystals that dont melt at room temperature, I would say re-a/b it.

As for the attempt to smoke it, I dont understand when you say "too much base", because sodium carbonate does not vaporize at lighter temperatures, so you cant be smoking it... I have a feeling maybe its your smoking method and/or other impurities in the dmt making it harsh. Thats why I would do the re-a/b on the product, as well as get a vaporgenie and a torch lighter for a smoother vapor and not nasty combustion of dmt.
 
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Ahhhhh ok!!!!... Well, swim will try this. (I TOTALLY spaced out of base/acetone problem!!)

What swim added to the d-limo will be evapped to end up with hopefully some additional fumarates. And then will try acetone from there..

And then swim will evap the FASW+NaCO3 solution, and then resoak all of the freebase dmt in vinegar, and then re-do from there A/B using acetone re-x'ing.

This makes SWIM think that Amor Fati's tek is only useful for pharmahuasca or bongs.
 
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Ok, swim just figured out an integral fact to this problem that swim overlooked and didn't know about until swim read a link in the faq about 'yellow goo'.

I always thought yellow dmt was n-oxide, while the clear was in-oxidized dmt.

It turns out that pure n-oxide is a goo at room temperature... and that heat oxidizes dmt during the extraction process..

Well, when swim was evapping the fumarate as well as the freebase dmt, swim was doing so over a hot plate set to low (but i guess not low enough).. At one point, there was enough heat that some wisps of steam came off the dish. This to me seems like the perfect condition to oxidize dmt.

And this explains why the naptha is yellow and the yellow goop did not dissolve after re-x'ing. Well, swim at least knows that the yellow goop is n-oxide and will scrape it onto some leaf and toke!

As for the rest of the madness, swim is led to believe that even dumping mimosa into a hot lye solution is overall not a good thing in terms of oxidization, and this is perhaps an explanation as to why the d-limo turned such a heavy yellow color, as well as the FASW being also colored yellow.

Whew. Well, at least swim knows that if he can't get crystals, he still has got some n-oxide to play with!
 
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IME dmt oxidation happens much less often than people suppose. It can happen that depending on how you evaporate it, you get an oil at the end, but if you recrystallize it, it comes out as crystal dmt. It seems small amounts of solvents + plant oils mixed with the dmt can make it stay as an oil and crystallize with more difficulty and make people think its n-oxide. But then with cleaning up and recrystallizing, one gets nice dmt crystals.

Yellow solvent is most likely other plant oils, specially if you had an impure product...

I would attempt to get crystals and yeah in the last case you can infuse herbs, but I would say you can probably get it done :)

BTW, heat to evap fumarates is no problem at all... better avoid heat when evapping freebase.
 
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::sigh::

Well the results of the fumarate evap turned out to be yet another bust...

swim scraped up an amount which equaled the mass of a quarter when flattened out from 1 wash of about 50-70 ml FASW in the d-limo solution (granted this was the 5th wash that this has undergone).

Then swim used 5 acetone washes (of about 3-5 ml at a time) on this mass, stirring it in the acetone among dissolving. The entire mass dissolved.

Now swim has a glass vessel with brown liquid (which swim accidentally spilled some on his arm, and when it evapped it smelled like straight impurities/vague citrus smell) and on the bottom is some cloudy whiteish liquid.. but no pure dmt-fumarate..

---
swim will now attempt evapping his FASW+NaCO3 solutions.
 
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I dont understand, what fumarate evap? Did you do a re-a/b on it?

when you say "amount which = mass of a quarter", its impossible to estimate because there can be different densities, which can vary a lot.

Then you say "1 wash of fasw in dlimo", but then you say its the 5th? So where are the other 4? and are these all your limonene pull combined or you still have to salt other pulls?

The spilling part is some weird detail in the story to make this whole thing more complicated :p

So again, did you redissolve everything where your impure alkaloids must be, in warm acidic solution, and re-a/b it?

You are really overcomplicating yourself, when something doesnt work, dont start doing a billion of improvised things and separating all sorts of parts that you have no idea what they are, because then it gets ever more complicated to solve what you're doing.

Redissolve, re-a/b, re-salt with FASW, evap, tell me what you have.
 
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Just to clarify:

Swim had some more FASW that Swim poured back into the yellow d-limonene. Swim separated the bottom layer and evapped it to get something that when dissolved in acetone, showed up no dmt-fumarate. This is all completely separate from what I already had problems with... Swim pretty much tried to do another FASW pull with the d-limo that Swim started with.

The other 4 washes are what became of the freebase (4 from Jorkest's tek), and the 5th one is just the attempt to see if there is more dmt in the d-limo... I guess there isn't.

All the other stuff that Swim has is still in the fridge.
 
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