Purification failures

[Du57mi73]

I cant understand what I'm doing wrong. I used to be able to produce crystal clear beautiful crystals. I understand WHY I'm getting yellower crystals. I know its because I'm reusing my naptha from previous pulls. But i am having multiple problems and was wondering what i can do to fix my problems.

The first problem im having is during freeze precipitation. I freeze precip inside of a mason jar. My problem is that when i do a freeze precip, im having large amounts of plant oils also fall out of my solution as well as alkaloids. Leaving my final freeze precip noticably more yellow than it should be. It comes out deep deep yellow. Not what i want. I was wondering if so much oil drops out because of the temperature? seeing as how i sit my jar in my ice cube bin in the freezer, and that low temp makes more oil fall out then normal? or i dont know. ive been chalking it up that since i keep reusing the same naptha that it just keeps building up with more oils than normal which is what causes this. I think i might be right on that, but if temperature makes a difference, maybe ill consider not putting it in the ice. I put it there cuz it finishes freeze precip in roughly 3 hours.

Second problem i am having is during re-x. I think im doing something wrong in this step. Ill put my dmt at the bottom of my jar, i heat up naptha, and then pour it into the jar by spraying it against the wall so as to not disturb the spice bed. I let the naptha sit for 2-3 minutes then pour it off. But the problem here is that no matter what, im never left with plant oils at the bottom. It seems the DMT absorbs just as rapidly as the plant oils and everything is absorbed into the naptha. i guess this shows that there is no lye contamination, but im looking to clean the oils out of the spice. So then i figure its fine, cuz some of the oils will stay in the naptha when i freeze it again. And it does, but no where near as much as id like..

Third problem is with a "defat". i do a mini a/b to try and remove the oils. I take 1 part vinegar, two parts water, and absorb all of my spice into it. Everything absorbs into it and it turns yellow, which i find strange, seeing as how oil shouldnt absorb into water. Anyway.. when its in the acid solution i would add clean naptha to try and grab some of the oils. This doesnt happen. It stays completely clear no matter how long i let it sit or shake it up. So then i remove all of that naptha, basify again, and then pull with clean naptha. When i do this the "yellow" follows the dmt and absorbs into the naptha(as it should, i suppose). This leaves me with an all white basic solution, and yellowed naptha, just like what i started with. No defat at all has occured.

This is what happens to me on a regular basis now. Is there something im doing wrong? i thought i fully understood the whole process but i guess not since there are a few things that still elude me, such as why doesnt the clean naptha on the acidic solution pull any oils? that doesnt make any sense to me at all. Its as if the "yellowing" is stained into the dmt or is maybe another alkaloid that follows the same chemistry rules as dmt, which is possible but i highly doubt, unless its n-oxide which i highly doubt.

Im considering freeze precipping in a flat dish like i used to. Maybe that will help with some of the yellowing as the oils will disperse and not concentrate themselves onto the layer of spice. And thats another thing. When i freeze it, all of the oils are on the very bottom of the jar, caking my spice together.

Can yall give me any tips or point something out that im doing wrong?

 

[arcologist]

The yellow 'oil' you are dealing with is not an oil but instead mostly DMT N-oxide. It is less soluble than DMT in room-temperature or colder naphtha but can still be dissolved with hot naphtha. Don't fret, this material is still active and can be easily converted to regular DMT if you can get some zinc metal dust.

Here's what I would recommend: get some zinc dust, dissolve all of your impure DMT + N-oxide in a minimal amount of vinegar, put the zinc dust in the vinegar, stir occasionally and let it sit uncovered (important!) for at least an hour. You should notice a color change from yellowish to clear. This indicates that most if not all of the N-oxide has been reduced to DMT. Now you can filter out the zinc, add NaOH and pull again with naphtha. The result should be pure white and a bigger yield than if you recrystalized.

In the future when doing an A/B extraction, after filtering out the bark and reducing the volume of the acidic solution, I would add zinc dust in a similar way. This will convert any N-oxide that is present in the bark to DMT and should increase your yield.

 

[Du57mi73]

I dont do a/b extraction, i just posted it here because i didnt know where else, and because i thought my third problem might be helped here.

I was reallly suspecting it was n-oxide but endlessness made me think that n-oxide is alot rarer than led to believe. haha. but ill try out the zinc. a question though, why would i put the zinc into a vinegar saturated solution, rebase it, then pull with more naptha, when i could just as easily add the zinc to the naptha. Does it react somehow? Whats the best way of procuring zinc metals? the zinc supplements i find are of zinc dioxide, which im guessing by basic chemistry that it wouldnt grab oxides if its already a dioxide. lol

how confident are you that this is n-oxide? have you dealt with this before? if this is the case i will definitely post before and after pics of a zinc reduction.

 

[DreaMTripper]

If its ACRB it could also be NMT..Also a yellowy oil..
What plant matter are you using and have you tried washing the solvent with basic salty water? If it doesnt cross over after washing its likely an alkaloid as archologist said above..
According to the wiki.. Psychedelic Compounds Chemical and Physical Properties - DMT-Nexus Wiki
DMT n-oxide "Insoluble in petroleum (naphtha) but appreciably soluble in petroleum which contains fats. Ghosal & Banerjee 1969"

NMT " Soluble to some extent in naphtha (not nearly as much as DMT). It seemed only partially soluble in warm acetic acid. It is likely soluble in xylene. (Source )"

I personally would love to have a combo of these with DMT but each to their own..

 

[Du57mi73]

Freebase, n-oxide, and nmt? How adventurous, I'm down. You need some jimjam with that there sammich?

I started thinking about n-oxide. There were things that happened during the extract that made me not believe it was n-oxide. The main reason was for the quantity of n-oxide. Its gotta be atleast 30% of my yeild. I didn't think the plant would have that much n-oxide in it. Plus I thought you needed heat to make n-oxide, hm. I guess the only way to figure this out is to add some zinc and see what happpens.

But other than that my steps seem fine though? K.

 

[arcologist]

You need to add the zinc in an acidic solution so that there are H+ ions to reduce the DMT N-oxide. It won't work in a solvent.

I recently did an extraction on ACRB where around 40-50% of the available DMT was the oxide, I was surprised at how much there was. It's probably variable based on the source material. N-oxide is very slighly soluble in naphtha, much more so in xylene. I think that most people that extract with naphtha don't pull very much anyway and so it isn't very often encountered. The above extraction was done with xylene.

You can get zinc metal dust on ebay. It is commonly sold as an ingredient in homemade fireworks and pyrotechnics. It must be the metal zinc, not zinc oxide or any compound of zinc. Fine powder will work better.

 

[Entheogenerator]

Ill put my dmt at the bottom of my jar, i heat up naptha, and then pour it into the jar by spraying it against the wall so as to not disturb the spice bed. I let the naptha sit for 2-3 minutes then pour it off. But the problem here is that no matter what, im never left with plant oils at the bottom. It seems the DMT absorbs just as rapidly as the plant oils and everything is absorbed into the naptha.

I've never heard of this method of recrystallization. I'm not sure that it would work... Here's how I've done it and heard of others doing it:
- Heat up DMT and naphtha in separate shot glasses in a sauce pan
- add just enough hot naphtha to dissolve all of the DMT (nothing left in the shot glass)
- let it cool for at least an hour or two, until it is at room temperature
- put it in the refrigerator for a couple of hours until no more impurities seem to be dropping out and it has dropped to the temperature of the fridge
- decant naphtha off of the impurities and evaporate or freeze-precipitate

What plant source are you using? It is pretty unusual to have bark that contains high amounts of n-oxide unless it has been stored for several years since harvest, but it certainly isn't impossible.

 

[Du57mi73]

My bark is good. I used MHRB. I stand by that.

Entheogenerator, what I do is the same thing as you except I use a thin jar(made for peppers) and re-x multiple puls at once which is hard to do in a shot glass. Lol. Its the same thing, just a tiny bit larger scale.

I think that since n-oxide is absorbable in fats that my normal clean naptha pulls weren't pulling the n-oxide, but when I reuse the naptha over and over it builds up some oils and that's what the n-oxide grabs onto.

Hm. Are there any regular uses for zinc? I'm kind of sketched about buying things online, especially stuff to make explosives. Haha.

 

[Cosmic Spore]

Hm. Are there any regular uses for zinc? I'm kind of sketched about buying things online, especially stuff to make explosives. Haha.

I ordered 1 lb of zinc dust off of amazon or ebay (forgot which). It arrived fine & I don't have any reason to think that purchase put me on a list. Haven't used it yet, waiting for a better pictoral of the reduction reaction, before I go for it.

I'm sure that there are legitimate uses for the zinc dust, even legitimate reduction reactions. (correct me if I'm wrong).

 

[Du57mi73]

Hm. Are there any regular uses for zinc? I'm kind of sketched about buying things online, especially stuff to make explosives. Haha.

I ordered 1 lb of zinc dust off of amazon or ebay (forgot which). It arrived fine & I don't have any reason to think that purchase put me on a list. Haven't used it yet, waiting for a better pictoral of the reduction reaction, before I go for it.

I'm sure that there are legitimate uses for the zinc dust, even legitimate reduction reactions. (correct me if I'm wrong).

I was thinking that the same could be said for rust removal but im probably wrong. Some acid solution, some zinc dust, and some elbow grease? lol. im sure just an acid solution alone is probably enough though.

Ill probably do a step by step when i do this reduction if it goes well ill post about it.

 

[Entheogenerator]

My bark is good. I used MHRB. I stand by that.

Entheogenerator, what I do is the same thing as you except I use a thin jar(made for peppers) and re-x multiple puls at once which is hard to do in a shot glass. Lol. Its the same thing, just a tiny bit larger scale.

I think that since n-oxide is absorbable in fats that my normal clean naptha pulls weren't pulling the n-oxide, but when I reuse the naptha over and over it builds up some oils and that's what the n-oxide grabs onto.

Hm. Are there any regular uses for zinc? I'm kind of sketched about buying things online, especially stuff to make explosives. Haha.

Hm. Maybe I misunderstood from what you wrote before. But yes, I would definitely recommend using fresh naphtha for your pulls, or distilling your used naphtha to remove anything that remains dissolved in it.

I too have purchased zinc dust off the internet without any problems. Zinc is often used as a propellant in model rockets. You could order some zinc, a model rocket, and perhaps a few of those little cardboard tubes that people use as "engines" for model rockets at the same time if you are really concerned about it...

 

[endlessness]

Is this from mimosa or acacia?

I think evidence for n-oxide being present in extractions we deal with here is scant to non-existing at this point... It was more of a theory than anything else... If you want to do the whole zinc reduction story, please have a `control group`, by separating half of your product and doing the same process as with zinc reduction except not adding zinc, to see if zinc is really doing anything.

How much naphtha per gram of impure DMT are you using for your recrystallization?

 

[Du57mi73]

When I re-x I use around 50ml per g.

And this is from mimosa.

Its like no matter what cleaning step I do, the "yellow" stays with the dmt.

Ill most likely buy a little zinc to test it. It can't hurt to try since the conventional methods aren't working for me.

 

[endlessness]

use 30ml instead of 50 and it should work better. Do a second pull on the goo with maybe another 10ml and freeze separately, to get a bit more out (but more impure)

The other possibility is that your naphtha contains a small percentage of aromatics mixed in which will dissolve impurities too well. Is your naphtha from a specific brand, or can you get access to it`s MSDS to see the contents?

 

[Du57mi73]

Am I supposed to heat the dmt when I re-x so that it kinda melts a little?

 

[Entheogenerator]

Am I supposed to heat the dmt when I re-x so that it kinda melts a little?

That's what I do... I don't know if it there is really any advantage to it though, aside from maybe making the DMT and impurities dissolve slightly faster.

 

[endlessness]

no need to melt the DMT, the warm naphtha will already do that.

 

[Tranzcentral]

Are you de-fatting your extract?

If not, that will be the result of oily crystals.

Also when you filter, and before you turn it to Base, try and decant your extract overnight, so the next day when you throw it all through the filter again, your getting rid of the finer sediments that would not collect in your filter papers the day before.

Those extra fine sediments hold oils, so if you dispose of them, you'll save yourself the trouble of having to do a re-x. For a re-x results in a slight yield loss, so why re-x if you can take more care in earlier steps, have very clean and pure spice, and not lose any yield?

 

[Du57mi73]

I should have put this in the STB section. I dont do A/B, i do STB. I put it in this section just because of the back salting step. Which, would technically be the same thing as a defatting step. Applying a clean solvent to it while its in the acid solution. Youd think that would grab all of the oils. But for me it doesnt do anything at all. As for filtering sedament, i dont do that because of STB. I actually think i wasnt doing re-x's right anymore. I wasnt getting the naptha hot enough. I did another re-x with hotter naptha than what i had previously heated it to and it worked drastically better. I just dont understand why the backsalting didnt clean out any of the oils.

 

[DreaMTripper]

Some of the resins/gums in plants are not soluble in naptha and are of a polar nature.
When using phyllodes a pre-wash with ethanol/methanol was highly beneficial it would be interesting to see if this also makes a positive difference with mimosa root bark. I dont see why not.
You stand nothing to lose, if it turns out it pulls a load of alks too you can always recover them from the ethanol.

Have you changed the temperature at which you keep the soup and solvent? Or how long you leave the solvent in?
Or all of the above? In this thread red yellow white spice whats the difference? - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus people mention they produce different colours and consistency with different temperatures and exposure time.

According to the nexus wiki NMT has been found in mhrb so its possible you have enough to colour the dmt and that you've pulled it because of the temperature if and the oils present in the naptha.
Simplexus here suggests using a high heat method ... Acacia simplex extraction, dmt/nmt separation - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

...

To obtain white fluffy xtals, and separate NMT from DMT you should do that way:
When you do your pull with naphta, you should do it at high temperature.
Put your basic solution in a 1L glass bottle and add 200-300ml of naphta.
Put the bottle in a hot bath with boiling water (be very careful, and let the pressure release from time to time). Shake the bottle, let the pressure release. Try to keep the temp as high as your hand can handle the bottle (I guess 45°C). When naphta and basic solution are at the same hot temp, there is no more pressure to release. You can shake it like hell, if your solution is well filtered, pH high enough, and temperature high enough, you shouldn't have big emulsion. Once well shaked, let the emulsion disappear, this can be helped by pouring some boiling water on the closed bottle directly on the emulsion (again be very careful to release the pressure). Once the emulsion is gone, pull the naphta out from the bottle, this should be done when all is still hot.

The naphta is now oversaturated and very hot, by cooling, dmt xtals should appear at room temperature.
Put the hot oversaturated naphta in a dish, cover it with plastic film (no evaporation) and let it sit at room temp. After only 30 min you should observe xtal formation, wait 3 hours or more until xtals stop growing. You can now pour the naphta out from the dish letting crystals dry.
It's better to reuse the saturated naphta for next pulls. Do pulls until there is no more xtals forming at room temp. Using 1L of naphta is ok but for 100g of bark, may be you can use less.
Once you collect a maximum of xtals, keep the naphta and let evaporate (or freeze precipitation). You should obtain an oily orange/brown goo which is nmt and other compound like betacarboline.