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STB recrystallization questions

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TheHappiestLittleNug

TheHappiestLittleNug

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Swim about to start the first pull of a stb tek and he was wondering what the most efficient method of recrystallization was in terms of yield preservation and naphtha recycling. If the lye mhrb solution is pretty thick will it affect anything? Its been soaking for a few hours now. Its one ml to gram of naphtha right?

Also does using xylene affect recrystallization? Swim only has a little naphtha left and swim wants as much pure dmt as he can get. Jungle dmt sounds frightening lol.
 
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Okay swim is done mixing the 400ml of naptha he had into the solution. Got about an hour before it separates so feel free to answer soon. Swim is thinking of going with the freeze precip for the first naptha then doing an entirely xylene one. Evap for xylene though, then recycle the naptha another freeze precip, xylene then on the third recycle combine them and evap everything. Then just keep going on with the xylene, anyone see anything wrong with this? Swim just going on chemistry instinct and hypothetical knowledge here

Edit: Is it okay to leave the basified solution out for 8 hours, maybe more, then go right back into extractions?
 
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Shit its been an hour and nothing has come to the surface. Swim tried to take some liquid from the top but it is just dark. He stirred it again and added more water and lye. The ph is still above 13 and it doesnt have the consistency of mud anymore. What should swim do he has 1.2 lbs of mhrb at stake here guys someone please respond! Anyone seriously
 
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always when you're in doubt, you have to explain more what you are doing.. for example, cant understand from your pics what kind of container its being done in, neither know how much lye/bark/water you used from the beginning. 1,2 pounds mimosa is something like 500g, correct? I know you already started but, you shouldnt make your first attempt with so much, better start with 100g and then if something goes wrong its not such a big prob.. But since you started already, check the FAQ, there's a lot of information that may help you there. and specify better the amounts you used.

400ml naphtha seems like a waaaaaaaaay too big amount of naphtha.. freeze precipitate wont work, you sort of screwed yourself up in terms of reusing this naphtha.. you are gonna have to evap it to, say, 50ml, and then into the freezer.. Its always better to make smaller warm pulls (like lets say 100ml for your amount of bark), and make many pulls, like 6, and each time sticking in the freezer, yielding the crystals next day and reusing naphtha, because otherwise its just too much and it will never be saturated enough for a significant amount of crystals to crash out.

so tell us the amounts of water/lye used so far.. maybe adding more lye only will help, maybe adding loads of salt will help, dont know.. give more information and better pictures :)
 
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I started with something like 2 liters of water and added 13 tablespoons of lye into a 5 gallon noncorrosive plastic drum. Then added the mhrb. Let it sit for 2 hours, then added the naptha. I think what happened was I made a giant emulsion because the layers wouldnt separate and I stirred it for a good 40 minutes. I made sure not to splash around or go to fast, but there was a point where the liquid layer and the muk sort of became one, this didnt bother me at the time because how was I to know they wouldnt separate. In retrospect they probably would've separated eventually, but I freaked and added say a liter of water mixed with I think 2 tbs of lye. I didnt have time to let it come to the top again so I added and stirred 300ml of xylene at a time into the mix and proceeded to get a couple of nice yellowish vials for freeze precip. Pics when my parents leave, but I took a look at the vials and there are large trails of white crystals running down the sides. Planning on pouring off the xylene and doing an evap while i run to the store and pick up more naptha. Ill get some pure dmt yet

Ahh to learn new things. Next time smaller everything

Oh I left out that after the naptha didnt separate I took a smaller jar and poured half a liter of basified solution into it and tried to do a pull with isypropyl (didnt separate) then poured it back into the mixture after the third pull. Will that affect anything it was 500ml? I would think 6 hours would be enough for it to evaporate but anythings possible I guess
 
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sounds like a huge mess what you did there.. you shouldnt start putting everything in if you cant get things out in the first place!

2l water for 500g mimosa is way too little.. the recommended amount is 1g:1g:15ml Bark:Lye:Water.. so in your case it should have been like 500g:500g:7,5 liters !!! So you see the difference, it should have been waaaay more water to begin with, thats why your layers are not separating

Mixing iso is a horrible idea, of course it wont separate, iso, like other alcohols, mixes with water, how were you thinking of separating it?! Now at least part of your dmt will refuse to come out because it will be in the iso+water layer

I would advise stop pouring things in like you are doing! Next time do it simple, use more water and lye, use less naphtha...

I dont even know what to say more.. I dont want to sound harsh but damn, man, your attitude in the extraction seem quite off! freaking out and adding more and more stuff, having problems that a quick look at the FAQ or other threads would help you solve, etc... You should do this more calm, read, if there is a problem let it stand and try to find out how to proceed, but dont go all hectic about it getting desperate and acting out of impulse


Maybe divide the mess you have in different containers, add twice as much water+lye as there is (pH 14), evap all the solvents you had mixed so far, recrystalize whatever comes out, and be more calm next time
 
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Damn it the lazymans tek I followed said for an lbs of mhrb I should only use 2 liters. Okay okay all I need to do is split it up, after I get more naptha, add enough water that the total would equal 7.5L, get the phs to 14, do a few more pulls and i'll have gotten most of it right? Wouldnt the iso evap regardless of bonds? Its been 8.5 hours now and I might have to let it sit around 11 hours longer before I start extracting again. Btw when dose the lye start breaking down the DMT?

I go by the live and learn view of life. Yeah I wasted a bit, but i'm hoping the sheer bulk of mhrb I used will balance out the mistakes I made. See next time i'll know that bigger is not better and that a large amount of naptha should be obtained beforehand and used in smaller proportions. My technique needs balance and rational.
 
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Ok my friend i see a few easy problems here. First you should let the lye water root bark mix sit for over night in your bottle. Second dont worry about the ph and all that as long as you used the formula: 200 ml deionised water, 5 g caustic soda, 20 g Mimosa hostilis root bark powder, 50 ml naptha. It makes no diffrence as to what amount you use as long as the ratio is the same. Personally I use 40g of mimosa. After you let the lye, root, and water sit over night add the naptha and shake shake shake shake. a good 5 min wont hurt a thing. next the mix will take a good day if not longer to seperate. BE PATIENT. and put the bottle containing the mix in warm water espcially right after shaking. If after 2-3 days there is still alot of imulsion you could add a bit more lye and shake for another min. let sit for another few days and ther will be a clear seperation with minimum emulsion. You dont have to completly wait for all the emulsion to clear up before taking some naptha off. just be sure you let the mix settle and you are geting 100% clear naptha.
 
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dont shake, it doesnt increase yields in SWIM's experience and it makes it nearly sure that there will be emulsion.. SWIM stirs strongly for a few minutes in round motions, forming like a whirlpool in the center.. As soon as he stops stiring it basically already starts separating, in few minutes its done.. SWIM repeats this a few times and it always separates fast... Then one doesnt have to wait for emulsion settling or any trouble. Just make sure pH is high enough

50ml naphtha pull per 40g mimosa will work of course but IMO its a waste.. This naphtha pull would be enough for 3-4 times the amount of bark, just make it warm and do more pulls. This way also one doesnt have to evaporate the naphtha and can stick straight in the freezer, and then can reuse the naphtha
 
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So far so good not much to report got another couple pulls in emulsion free, one more questions though.

In a freeze precip how do I get the crystals out of the jar before they melt back into the solvent? Just scrape like the wind or what?
 
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1 Remove the jar from freezer and quickly but carefully empty out naphtha (the crystals should stick to the bottom and sides of the jar).
2 Replace the jar lid and put back in the freezer upside down (at an angle) for half an hour.
3 Remove the jar from freezer again and empty out any residual naphtha.
4 allow the crystals to air dry (perhaps using a fan).

8) yum.
 
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transitory said:
1 Remove the jar from freezer and quickly but carefully empty out naphtha (the crystals should stick to the bottom and sides of the jar).
2 Replace the jar lid and put back in the freezer upside down (at an angle) for half an hour.
3 Remove the jar from freezer again and empty out any residual naphtha.
4 allow the crystals to air dry (perhaps using a fan).

8) yum.
Click to expand...

So... I did that now im drying the crystals and they are melting? Heres a pic

Looks more like orange ice

Edit: Wait didnt turn it upside down. Fuck everything I try turns to shit. Even my evaps havent produced any crystals yet all im getting is lots of yellow solvent and nothing in it. Pic

Naptha
 
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