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The Big & Dandy N,N-DMT Extraction Thread - Elves are watching

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I've collected more info from my friend. He's been following Lazyman's tek mostly.

He mixed 1lb powdered/finely shredded MHRB, roughly 1/2 lb pure NaOH and some distilled water in a one gallon glass growler, mixing it into a black sludge and letting it sit for a couple hours. Then, he poured a couple hundred mL of naptha into the jug, swirled it around gently until it was mixed in with the sludge, let it sit for a couple hours and poured the naptha off.

The first pull he started late at night and collected the next morning. This was a couple hours after mixing the initial lye-water-mhrb. The second pull he did after collecting the first and left in for a couple hours. I believe he's done 2 or 3 more since then, each with a fairly small amount of naptha.

On his first freeze precip attempt he had put the first batch in, then took it out to add the second batch, then took it out again less than 24 hours later. His freezer doesn't have temperature settings and it's a pretty basic food fridge/freezer unit, so I don't know how cold it will get. He's got the naptha in a pyrex baking sheet (like the kind you make brownies in, not sure exactly what they're called) covered with clingwrap and sitting in his freezer.

I see 3 potential problems, one of which seems less likely:

1) the lye-mhrb-water step failed and there's no dmt freebase to collect yet. This seems pretty unlikely, as 500g of lye ought to be plenty to make that mixture hella basified. If all else fails, though, I'll tell him to get some pH papers that measure up to 14 and make sure the pH is 13-14 (that's the target range, correct?).

2) the naptha step failed and there's not much in those pulls. Maybe he should try shaking it well and just letting it sit overnight to settle the emulsion, to make sure it's getting a proper 'pull' through the sludge? He's just swirling the upright jug, so maybe it's only collecting whatever freebase happens to be floating near the top of the solution. I had the idea of turning it upside down and back up again slowly a couple times to let the naptha run through the whole mixture as it floats to the top each time, but for all that the growler cap is secure and watertight in theory, turning a mixture of noxious chemicals upside down is kinda scary and we didn't want to just try it on a whim. Could this step be where he's going wrong and if so, recommendations on good tricks to make sure it mixes properly?

3) there's a decent yield of freebase sitting in that naptha but either his freezer isn't cold enough or he just didn't leave it in long enough. This one is easy enough to diagnose: I told him to leave it in for a solid 36 hours with the freezer closed the whole time, and if that fails to produce results then he's just gonna evaporate the pulls he has now to see what's in 'em.



Adrian: how much volume do you start with? He used a pretty small amount, just a layer of maybe an inch or two over the top of the lye water.
 
^Yeah dude, w/ 500g of lye you've maxed that shit out. I mean, unless he was using a ridiculous amount of solvent, like 15 liters of water or something, which I assume wasn't the case.

I would combine the pulls, then evaporate the naphtha to half its original volume under a fan. Then throw it back in the freezer, and just let that sucker wait in there and really lose energy. It takes time to really chill something thoroughly. Give it a 72 hours or so.

Is the freezer cold enough to freeze ice cream HARD? Like where you have to warm the spoon up under the tap to break the surface? That's how cold it needs to be, really the colder the better.
 
I'm not sure if the freezer is cold enough or not... Maybe we'll have to get some ice cream for testing ;)

Definitely no ridiculous volumes like that - probable a couple liters, enough that along with the mhrb and lye the mixture fills about 2/3 of a one gallon container. 500g should be more than enough, and probably even by the first pull a couple hours later most of the dmt was freebased, I'd imagine, since he started with powdered/finely shredded mhrb.

I'm starting to think he may just be best off evaporating the naptha, and if that fails then maybe his naptha 'swirling' technique is mixing insufficiently.
 
Try mix your pulls more with the lye mix. It sounds kinda like you are just swirling it for a lil while and then not touching it again. I tend to mix it for round 5 min. straight when I first put the nonpolar layer in, and then mix it a couple times over the next few hours (or day or so) to make sure everything gets mixed together.

And I'm not exactly sure how much nonpolar solvent I use, maybe round 100-200mL, I can't really envision how much naphtha that is you are talking about though, what the diameter of that container?

My freezer is by no means all THAT cold though. I usually make sure to eleiminate a good amount of the solvent before putting it in there to ensure that it precipitates.
 
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i agree with adrian.
I agitate the bottle at least 3x at ~1 minute each time. (waiting for the naptha to seperate before agitating again)
And instead of swirling, tip it end to end. You really want the naptha to go through all of it.

Also how much lye did you use? In your post it says both 1/2lb and 500g. If you only used a 1/2lb of lye for 1lb of MHRB that isnt enough, you want 1g lye/1g MHRB.

Dont worry you havent wasted the naptha or ruined anything. You can reuse that naptha as its probably not saturated at all.
In fact i resuse naptha 3x before getting rid of it.

As for the amount of naptha to use. I also dont know how much, i use, i just eye ball it now and dont remember the amount i used when i first started.

Check out Nomans Dmt for the masses Tek (its on erowid and a million other places). His measurements are what i originally used and it worked great.
 
^^^ Yeah, I think it's actually half a pound, had a brain fart and mixed up pounds and kilos. Fuck measuring things in pounds -.-

Is a 1:1 ratio really necessary for such large quantities? The example quantities in Noman's are much smaller, like 50-200g at a time of bark. Half a kilogram of lye for a couple liters of solvent seems like.... a lot. Lazyman's tek says to use 200-250g lye for 500g bark.

Reading around elsewhere, it seems that freeze precipitation works like this: the solubility of the DMT in naptha is a function of the temperature of the naptha, with lower temperatures having a lower saturation point. 100% saturated naptha would theoretically 'bang out' at least a little DMT if its temperature were dropped just a tiny bit. Is that right? If it is, I assume that means that, in terms of freezer temperature, the colder the better, but a less cold freezer would still produce *some* yield if the naptha is sufficiently concentrated. It'll just leave a higher amount of DMT still dissolved in the naptha than a colder freezer would have, right?
 
He's got some more pulls that have been much more thoroughly mixed through (swirling the jug and turning it end over end to let the naptha pull through all the material repeatedly, at least a few times over at least a few hours), and is trying to evaporate off as much of the first couple pulls (which is about 1 quart total volume, or was before he started evapping).

Random question - any recommendations for a suitable container to evap in outside? Right now he's got it in a little glass baking dish with cheesecloth tied over the top to keep insects/twigs/etc. from falling in (it's outside in his yard since he lacks a properly ventilated indoor workspace to evap off that much naptha safely). We've had a hard time thinking of better methods - the cheesecloth tied over the top method isn't exactly perfect, but we can't leave it uncovered or all sorts of random crap will get in there. Some sort of container with a mesh or other bug-and-plant-bit-proof screen would be ideal but I'm drawing a blank as to what sort of container would fit the bill.
 
I usually leave it inside next to a window with a fan blowing over it pointing outside, and that's always been fine, the vast majority of the fumes go straight out the window.

You can also buy a circle screen that will fit right over the glass dish in the kitchenware section of most grocery stores that is very fine, enough to keep unwanted stuff out, but more conducive to evaporating.
 
After evaporating off all the naptha, my friend says the end product is still somewhat moist. Is this excess plant fats/oils? If so, I think we may try dissolving it all into a small amount of warm naptha, then putting it in the freezer... If we get close to full saturation with the warm naptha, even a not-so-cold freezer ought to be enough to precipitate out a decent proportion of the yield, right? Also - water condensation in the freezer is not a problem, is it?

Aside from recrystallization using a small amount of solvent in the freezer, is there an easy purification tek that doesn't reduce yield of actual DMT by too much?
 
I now have much more detailed info. It's waxy and has that darker tannish-brown jungle spice color, but it seems to smoke just fine - it's just sticky and annoying to store and work with.

The only stove he has access to is gas burning. My thought was to get some water up to a simmer, put a small amount of naptha in a glass container of some sort, turn off the gas flame and use a hot water bath to heat the naptha up a bit. Then dissolve the material in it and leave it out for a half hour or so to cool slowly a bit, followed by a couple hours in the fridge, followed by an ice water bath (maybe in the less-than-optimal freezer for good measure?). That should yield some little chunks of relatively pure dmt as precipitants, correct? Pass it through a coffee filter, thoroughly dry the yield and voila. After all his pulls are done, he can take all those small recrystallization pulls worth of naptha and evaporate them, then do the process one last time (maybe more if that 'last time' produces significant yields). Am I on the right track?
 
lewk said:
After you do a couple of pulls, if you want to decrease the amount of Naptha you gotta put in the freezer is that when you evaporate it off?

Does this loose any DMT in the process?
and do you do it just by leaving it in a cool/dark area and let it evaporate slowly, or can you heat it to make it evaporate faster?
Click to expand...

Sorry, still looking for an answer

If you've got your DMT solvent, and you evaporate most of it before freezing the crystals is this essentially evaporating the DMT floating around in the solvent?

or does it just evaporate the solvent, and leave the DMT behind?
 
lewk: the DMT does not evaporate. It is far too heavy. You're just increasing the concentration by evaporating off some solvent.

Careful using heat, naptha is highly flammable and the vapors are intoxicating and not so good for you. The plus side is that you can get higher concentration with warmer solvent, which means more will 'crash out' after you cool it down in the freezer. I've always just put the naptha in a shallow, wide container like a baking sheet and left it by a window with a fan blowing over the top. It evaporates fairly quickly this way.
 
solistus said:
^^^ Yeah, I think it's actually half a pound, had a brain fart and mixed up pounds and kilos. Fuck measuring things in pounds -.-

Is a 1:1 ratio really necessary for such large quantities?
Click to expand...

The only thing necessary is a very high pH, as long as that requirement is satisfied then you're good. :)

Using a 1:1 ratio just allows you to avoid having to crunch through a ton of annoying stoichiometric bullshit, that isn't really necessary in this situation anyways.
 
Cheers solistus, that makes sense.. things should be alot easier dealing with half the solvent
 
IGNVS said:
take ten and a half cups of that good ol HtwoO
and throw it (by jently pouring) in a gallon sized jar of your glass choosing

followed (at your leasure) by adding a half a cup of granulated lye "crystals" (pure btw, nothin in them, i know u know but just gotta throw this phrase in the tek to make it legit for the other readers, lovin you btw)
Click to expand...

I have a friendly bit of advice concerning this step listed above.

To avoid pH spikes and potentially harming your material. Instead of adding NaOH to your H20/MHRB mix, make your base water first, let it cool and when it is cooled and all mixed well, THEN add your powdered MHRB. It has worked well for me, and advised to be done that way on many different teks.

Also when you purchase lye, or drain opener etc, make sure and look on the package and be sure it reads 100% NaOH also called Sodium Hydroxide. If you buy the type with aluminum in it or anything that is not 100% NaOH, then you run the risk of getting impurities, not to mention possible fatal consequences when smoking the final product.

With that being said, be safe and careful and always WEAR PROTECTIVE EQUIPMENT, especially when working with NaOH as it can cause severe burns.

- Noddy
 
What happens if you were to evaporate off all the Naptha before doing the freeze precipitation?

Is all the DMT essentially evaporated aswell?
 
Nope the DMT can't evaporate, you'd just be left with a less pure product than if you had done a freeze percipitation
 
lewk: The DMT will be left over, along with all the impurities. The main points of freeze precipitating: 1) it's faster, and 2) you theoretically get most of the DMT and almost none of the impurities to 'crash out'. When you evaporate the solution, the *only* thing you're losing is the naptha. Everything that was dissolved in the naptha will stay put.

others: My friend took the waxy residue and redissolved it in a small amount (maybe 20-30mL or so) of naptha, heated in a hot water bath and then cooled in the fridge, then an ice and salt water bath in the freezer. This caused a good amount of DMT to crash out as a slightly yellowish white solid, but there was also a small amount of dark brown material that formed on the very bottom of the container. After pouring off most of the naptha, he redissolved what crashed out into a smaller amount, poured the result into a shallow pan and set it under a fan to evaporate.

What was that dark brown material? Our theory was that he did *too* good a job supersaturating the solvent so some of the plant impurities also crashed out. If that's the case, using more naptha should prevent the impurities crashing out. Is that what's going on, or did he do something else wrong? The material hadn't finished drying last I heard, so he's not sure if it will come out with a waxy or powdery consistency, but if it's still waxy, what would y'all recommend? The naptha was a deep/dark amber, like an ale, before the recrystallization, and after straining all the precipitates out, it was a much lighter amber, more like a lager.
 
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