DMT acetate crystals?? (ACRB)

[dcl525]

Finally broke down and made an account... and I need a lil' help...


First ACRB Extraction:

250mg ACRB extracted (A/B) using naptha as the solvent, my noob ass ends up with VERY yellow naptha with bubbles of fatty garbage on the bottom of the jar. After a few mildly successful freeze precipitations/filters and scraping some rather inconveniently shaped mason jars, I ended up with a few grams of a sticky, half decent DMT freebase (brownish-yellow coloration) and another couple grams of a substance that ranged in consistency from a viscous oil to a hard wax like substance. Bioassay of both revealed that they were both around the same potency, no crystalline beauty but functional spice.


SO. That was a week or so ago. I decide I'm not happy with the end result I got and get to researching the best method to go about washing my solvent in order to yield something closer to crystalline instead of this wax and goo and am determined to escape being chalked up as just another ACRB extraction that yielded gooey shit.

I dig up the ending of some TEK that involves transferring the DMT to an acidic solution from the saturated solvent, conversion from DMT acetate (in acidic solution) to DMT freebase using Sodium Hydroxide and pulling the freebase from the solution with fresh solvent.

However I get excited and remember how I had heard of salt being used in early washes before the initial pulls, and decide COMPLETELY WITHOUT THOUGHT to introduce that into this process. This is not like me and I am usually very calculated, very thorough person; sometimes to a fault. But for whatever reason I decided to use salt in the acidic solution, 40g of water-softening non-iodized salt.

If you can believe it, something went haywire after this haphazard decision. I did some quick bullshit chemistry and calculated that NaCl, being polar in nature, will stick with the acidic solution after addition of base. The DMT acetate will be converted to freebase and pulled with fresh solvent and my thinking was that the NaCl would remain in the acidic solution, due to its insolubility in naptha.

If you haven't already realized how careless and stupid that decision was, let me elaborate further. I ended up with naptha that was crystal clear, saved the dirty yellow naptha for further pulls of this nature and set the clear naptha to evaporate. Much to my delight I return several hours later and the dish is covered in a white powder and some crystals. Ecstatic, I decide to begin evaporating out the rest of the solvent, and end up with a large amount of crystalline white (what I thought was) freebase DMT. Half the solvent is evaporated before I get around to taking a closer look at it, and I'm skeptical of it's appearance. It's just too white and too perfect, something tells me that I slipped up somewhere and I immediately think salt. SO. I quickly perform a few solubility experiments and find ZERO solubility of the salt as well as the lye that I had used in naptha. Relieved by this, I test the melting point of the compound and find that I can't get it to vaporize. At all. No matter how much heat I use. It just starts popping around and sizzling.

This tells me that I either somehow have managed to evaporate DMT acetate from naptha, which I thought was impossible due to the salt forms of DMT being insoluble in any NPS... or that the salt reacted with the DMT or sodium hydroxide and yielded some strange chemical that crystallizes similarly to DMT.

What the hell is going on here? It's actually driving me crazy. For all I know I could be scraping and drying god damn SALT. Both scenarios I laid out are equally unlikely in my eyes, but like I said I didn't do my full research this time around and the universe showed me, again, exactly why one should never skip out on research when it comes to something like this.

Any input would be greatly appreciated for this hopeless newcomer!

EDIT: Forgot to mention that this crystal that I'm left with after evaporation is totally water soluble. Just to add to the confusion..

 

[slewb]

I'm thinking the bubbles of fatty garbage you describe at the beginning sound like they were probably basic solution that somehow ended up in your naptha. Next time decant naptha away before freeze precipitating.

What you ended up with is probably salt and/or lye. I am confused though... did you ever add the sodium hydroxide to the acetate solution, or just salt? If not I am guessing the naptha pulled no DMT, and what you should do is go back, basify the acetic acid solution, and pull with naptha. Make sure there are no blobs at the bottom this time too.

 

[BongWizard]

Redissolve your spice in warm naphtha and do a mini a/b and pull with nps to yield a higher purity tryptamine fraction (white waxy crystals from freeze precip).

 

[dcl525]

Thanks for the speedy replies guys

I really don't think that I carried any of the basic layer from the initial A/B over into the solvent, however I can't say the same for water/acetic acid from washes of the solvent. My thinking was that, and reinforced by a method I have read in more than one place, I would transfer/convert the DMT freebase into an aqueous acetic acid layer, effectively forming DMT acetate, and then basify back to a pH of around 11 and pull the freebase from the aqueous layer with fresh naphtha. Sounded logical. Anyway the small bubbles of what I thought were plant lipids or something are likely just water trapped at the bottom of the solvent. That I was able to figure out relatively quickly.

I did basify with sodium hydroxide, however directly before I added 40g NaCl in order to prevent emulsion (I guess that's why I did it, this is the only part of the process where I won't let myself off the hook, I didn't research enough). This addition of sodium hydroxide, maybe too much, reacted with the acetic acid in the solution and gave me a totally new compound...

Sodium Acetate!

After catching up on my chemistry and reading up a little more closely on ionic bonds, it occurred to me what likely happened and it wasn't too difficult to figure out where to go from there. I initially thought that the free sodium and chlorine ions were the culprit and what I had left was some Frankenstein molecule that crystallizes like DMT but is virtually inactive. I also thought I might have a compound like sodium chlorate or disodium oxide or some other result of a reaction between the chemicals added to the acetic acid solution. I also thought maybe the salt I used is impure, or the naphtha I used is impure, but a quick look at their MSDS told me otherwise and solubility experiments completely removed their possibility of being a contaminant.

SO... The question remained, just what the hell is this stuff?

"For laboratory use, sodium acetate is inexpensive and usually purchased instead of being synthesized. It is sometimes produced in a laboratory experiment by the reaction of variable concentration acetic acid, commonly known in its 5–8% solution as vinegar, with sodium carbonate (washing soda), sodium bicarbonate (baking soda), or sodium hydroxide (lye). Any of these reactions produce sodium acetate and water."
--https://en.wikipedia.org/wiki/Sodium_acetate#Preparation

Completely and utterly useless. But it crystallizes just beautifully. Let me be the only sodium acetate cautionary tale, this confused the living hell out of me. I could not figure out what this stuff was. The acetic acid and sodium hydroxide and salt are all polar and all insoluble in naphtha so nothing was lining up. It made no sense to me that there could be anything other than plant alkaloids in the solvent. I guess we all know that research is the name of the game, I'm just hoping this stuff didn't end up in anyone else's spice without their knowledge. This sounds like a fairly easy mistake to make. My yields were also huge, about 200% what they should have been. That was another indicator of what I had done wrong.

I am usually a pretty well read, cautious and thorough person in this area. I'll chalk this one up as lesson learned!

Thanks again for the quick replies gentlemen, you rock! :thumb_up:

 

[FLeP]

So you're telling me that if I add lye to vinegar I'm going to get sodium acetate? I thought most ACRB extractions begin with an acid soak and then lye is added to that solution?

Going to have to test my last yeild now. It's over %1 so now I am worried. Should have paid attention in Chemistry.

 

[FLeP]

Is this really occuring when people use Cyb's tek? Does anybody else have any experience with this happening?

 

[dcl525]

This occurred during my extraction because I added salt during a wash stage, not to the basic soup.

Don't worry, I have heard great things from Cyb's salt TEK, I highly doubt anyone else managed to screw it up like this!

 

[FLeP]

Ok, sweet. Just sent my buddy camping with my first ACRB yeild so I was a little concerned. Thanks for your reply.