Purest spice yet

[OrangeEnergy]

It's so white it hurts my eyes!!!

I need to figure out how to make that happen! I usually just scrape the top to get the white crystals first, then do a heavier scrape with more force to get the yellow and the goo. I'm getting nicely resolved crystals by cooling to room temp, doing the fridge for an hour wrapped, and then the freezer for 24 hours wrapped, but still the yellow whether I use naphtha or heptane.

 

[Jees]

Indeed very white.:thumb_up:
What was the soup temperature while making that pull please?

 

[Pandora]

That pic is enough to make a stalwart psychonaut's mind drool.

 

[Jees]

Was at room temp, which would have been around 17 degrees. Warmed heptane in waterbath that I could keep my finger in. I did 3 agitations before separating.

Thanks.
Got yellow with pulls done at soup temp at 50degC (122F), with ordinary naphtha and all pulls combined to freeze.

That pic is enough to make a stalwart psychonaut's mind drool.

Drool generator it is :surprised

 

[Toshido]

I really want to try and grow some BIG crystals.

I wonder what vessels would promote the best kind of large crystal growth? Maybe a round bottom? Of course it would be difficult to take pictures or scrape out. But some kind of pyrex rounded bowl would hopefully yield what I'm talking about?

The crystallization dish I have is flat on the bottom but is slightly concave in the center, which pushes crystal grown more out towards the perimeter than it does in the center.

I'm sure this topic has been discussed amongst xtal aficionados.

 

[Toshido]

If I manage to grow a big one I'd leave it in there and mount it on my wall :lol:

Would be dope to trap it in glass or resin and make a dope DMT wizard staff/walking stick with it.

 

[Hyper Turtle]

Afaik, having a well shaped seed crystal (or a few) helps, and slow cooling/evaporation is key to growing large ones.

 

[Voidmatrix]

Here are some posts on obtaining bigger xtals.

Growing big crystals - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

Warm Evap = Larger Crystals? - Welcome discussion - Welcome to the DMT-Nexus

One love

 

[Jees]

OrangeEnery, please report on the next pulls and yields.
What kind of base was used?

I suppose this very white was mainly due using heptane and pulling at room temp.

Considering the pull volume to be way lesser than the soup volume, I guess warming the heptane ain't doing that much as it must come to a temp equilibrium immediately when mixing in the soup. I really can't wrap my head around the idea of a warmer non-polar pulling a colder soup. I know it's said here or there. Maybe I'm missing something?

 

[Jan e Kharabat]

I did a couple of mini A/B's and then recrystallized with heptane and ended up with this beauty! I think you have to use the right kind of vessel and reach the right amount of concentration so that the DMT doesn't fall out to soon as the solvent cools down to room temp. I let it stay at room temp for about 12 hours, then put it in the fridge for another 12 hours and then in the freezer for another 12.

 

[Toshido]

Dear lord you two are getting some nice crystals... what am I doing differently?

Dasein, take a look at my TEK, I am still running experiments on the same bark source, but no pure white spice. Also, what kind of dish is that in your photo?

Widderic's TEK

Orange Energy and Jees, regarding heating soup, I was directed towards this thread, which is also in my signature.

Heat your soup!

Also, based on this video (at least in the case of 100g Aluminum Potassium Sulfate Dodecahydrate and Water) you want to dissolve in 800mL of water because it grows larger crystals. Depending on it's solubility, polarity and ionization I doubt it has anything to do with DMT solubility but here's the video anyways.

[YOUTUBE]

Part 1 - Growing a seed crystal
Part 2 - Growing a big crystal

It explains that if our solution is too concentrated, it will grow many crystals far too rapidly. Now, I'm doing five 50mL pulls from 100g MHRB for a total volume of 250mL, that I then fast evap down using high heat to 50mL, and then I cool to room temp, then fridge, then freezer (inevitably disturbing it obviously before final freeze precip). My yield is 1.4 percent currently so that's .7g per 50mL solvent. I'm wondering if going straight to freeze precip while 250mL of solvent being in the dish will yield larger crystals, but I've found that even with 100mL of solvent, I have crystals floating around that never resolved.

This is turning out to be quite a resourceful thread that will surely be dug up again and again.

 

[ABe©eDarian]

Those are some really gorgeous crystals !

 

[Voidmatrix]

Eh,this one is appropriate too.

just some xtals - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

One love

 

[Jan e Kharabat]

Dear lord you two are getting some nice crystals... what am I doing differently?

Dasein, take a look at my TEK, I am still running experiments on the same bark source, but no pure white spice. Also, what kind of dish is that in your photo?

I don't measure anything when doing DMT extractions. But you learn to figure out when something's not ok. For example, if you dont use enough lye you'll get emulsions and if that happens, just add some more lye! Same goes for the amount of solvent and temperature etc. I usually keep the soup in a water bath while doing the pulls and usually its around 70-80° but again, I dont measure very often! During the extraction, I just pull whatever I can and then do a clean up afterwards. Last time I used benzoic acid to crash out DMT benzoate from heptane and used the same heptane to pull more DMT, I did around 8 pulls in like 5-6 hours and completed the whole extraction in a single day (I usually take a month or so...).
For clean up, you can do mini A/B a couple of times. Dissolve the freebase in acidic water (or just water if its in salt form), add some lye, pull with heptane, shake as much as you want, there wont be any emulsions! Usually you see a layer of snot between the heptane and aqueous layer, that is usually a mix of DMT and plant fats etc. Depending on the amount of DMT, you will need 2-3 heptane pulls to get everything out. A thin oily layer will be left swimming atop the aqueous layer in the end, that is not DMT! In the end you can drop a tiny bit of lye in there to see if there's any more clouding, if so, you didn't use enough lye! If not, you're good! dumb the entire solution, clean up the bottle/vessel and do another cycle. You can crash out the DMT from heptane with benzoic acid, or freeze precipitate. After 2-3 cycles, you will have very very pure DMT.
Next comes the matter of white and yellow... So, while in the beginning, the yellow/oily substances can be impurities mixed with DMT, after the purification steps, you can still end up with yellow waxy stuff but that will be pure DMT. In my experience, if you do hot pulls and drop them on a cold dish, the DMT starts to crash out too soon. To test this, you can do a hot pull, drop it in a dish, leave it for 30-40 minutes, then pour off the solvent in another dish, let the first one dry, you will see an oily layer at the bottom. You can scrape it off and try it, it will be very active! So anyways, in the final step, do room temperature pulls! put all the heptane in a dish and leave it at room temp for 12 hours, then either pour off the solvent in another dish and collect the pretty looking crystals and precipitate the rest seperately, or put the same dish in the fridge for 12 hours, then freezer for another 12.
Aside from that, I think the vessel needs to be small enough that the solvent makes around... one inch layer at the bottom. The thinner the layer, the lower the height of the crystal (as far as I know, the crystals don't grow above the solvent surface). I usually use a small pyrex dish with a flat bottom, but this time I used an evaporation dish but any pyrex bowl would do fine!

 

[Toshido]

Ok, I believe I've got the gist.

When I do re-x's I wait for the heptane to cool a little while so that the impurities have time to settle to the bottom and then I decant into a final dish to crystallize, giving whiter crystals. I could be doing the same with my initial pulls from extraction, I don't know why I never thought of that, I guess because I had re-xing in mind from the get go.

The crystal size growth as it pertains to solvent height also makes sense, it won't continue to grow out of solution for obvious reasons. So a rounded bottom makes sense for achieving a larger crystal directly in the center.

I'm a bit confused as to room temperature pulls though. I have my acidic solution at 70C and when I basify the solution it stays at 70C. I add room temp naphtha and immediately mix, settle, pull. Did you mean let those pulls that I collect into a dish cool to room temp? Or let the basified solution cool to room temp and add room temp naphtha? Was confused there.

Anyways, thanks for the response.

Eh,this one is appropriate too.

just some xtals - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus

One love

And true, definitely the mega thread, although I found people didn't really go super in depth with their process. It was cool finding Phlux's old DMT Tek though. He had good results but would use xylene and sodium carbonate to make DMT fumarate and then convert to DMT freebase. Was cool to see a TEK done that way.

 

[Jees]

When I do re-x's I wait for the heptane to cool a little while so that the impurities have time to settle to the bottom and then I decant into a final dish to crystallize, giving whiter crystals...

Not "impurities" damned why is this such a hard ongoing hoax? Say: oily DMT. :thumb_up:

You're right, let the heptane settle and cool off, give that time, possibly to the brink of seeing little crystals forming in the milk. Decant and freeze the decanted milky heptane. Repeat the process if wished. One should get a 1% yield of whites this way, or at least white enough to be called white.

 

[Jan e Kharabat]

Like I said, the yellow oily stuff is not just impurities, during the main extraction it is a mixture of "impurities" (let's call it "the other stuff" ) and DMT. But if you do a couple of mini A/B cycles and still end up with yellow waxy stuff, it is most certainly all DMT! You will also notice that the oils from initial extraction smell and taste different and if you vaporize isolated oil, it wont absorb in your lungs (it probably burns instead of vaporizing). But in any case, the yellow is not necessarily impurities!

What I meant by pouring off the heptane to see the oily layer was to show that that oily/waxy layer is also DMT and that the different color and consistency may have to do with how the molecules arrange themselves i.e. if it is crashing out too soon, it may form a yellow wax but the same wax can turn into glittery white crystals under different conditions of crystallization.

About the room temp pulls, I meant that specifically in the case of mini A/B. For the first cycle or two, you can do warm pulls, no need to warm the soup, just add the lye and it will heat up, that's enough heat! for the final cycle, you can dissolve the lye separately in water, let it cool down a bit, and add that. You don't need a whole lot of lye in the mini A/B cycles, just enough to convert all the DMT to freebase and some more so that the layers separate easily. So, for the final cycle, keep the soup at room temp or at least below 45-50. Add the naphtha, shake, pull, collect all the naphtha in the crystallization dish and let it stay undisturbed at room temp for 12 hours, under right conditions, you will have nice big flowers just after 12 hours at room temp.

 

[Toshido]

Not "impurities" damned why is this such a hard ongoing hoax? Say: oily DMT. :thumb_up:

I'm only part of the hoax because every single person on the Nexus seems to call it something else so I don't know what to call it. Fats, lipids, oils, impurities, polymorphs, goo, jungle spice, jim jam, pure dmt, waxy dmt. Can we get a sticky thread for this?

But yeah here's my re-x process decanting from 100mL beaker to 100mL beaker to 100mL beaker etc. I understand I should save that "gooey oily dmt" but it's so hard to remove from the beaker I ended up just.... washing it down the drain.... don't kill me.

 

[Hailstorm]

The truth is that yellow can indicate many things. It could be some junk extracted from the bark. It could be DMT N-oxide. It could be thermal decomposition, which can change the molecule in unpredictable ways – for example, it can fuse two DMT molecules together, forming a dimer; this seems to happen more readily if the temperature and pH are high (no need to go above pH = 12).

Only one observation does not seem to be disputed by anyone: white DMT is usually clean. So I always go for white.

In your case widderic, the initial extract seems already quite yellow. It is hard to say why. Perhaps you should try a defatting step – just "extract" your acidified mixture using the same technique but before basifying it, to see if that "extract" (which should be free of DMT) is yellow or not. If it is yellow – congratulations, you have removed an impurity, or perhaps your NPS is dirty. If it is colorless and the yellow color only appears after basification – I'd make sure your NaOH is reagent-grade, and try lowering the extraction temperature to see if the root cause was (oxidative) thermal degradation.

 

[Loveall]

The truth is that yellow can indicate many things. It could be some junk extracted from the bark. It could be DMT N-oxide. It could be thermal decomposition, which can change the molecule in unpredictable ways – for example, it can fuse two DMT molecules together, forming a dimer; this seems to happen more readily if the temperature and pH are high (no need to go above pH = 12).

Only one observation does not seem to be disputed by anyone: white DMT is usually clean. So I always go for white.

In your case widderic, the initial extract seems already quite yellow. It is hard to say why. Perhaps you should try a defatting step – just "extract" your acidified mixture using the same technique but before basifying it, to see if that "extract" (which should be free of DMT) is yellow or not. If it is yellow – congratulations, you have removed an impurity, or perhaps your NPS is dirty. If it is colorless and the yellow color only appears after basification – I'd make sure your NaOH is reagent-grade, and try lowering the extraction temperature to see if the root cause was (oxidative) thermal degradation.

I mostly agree, but in my personal experience it is usually DMT aggregation causing the off white color. I don't think N-oxide has been detected in a normal extraction.