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purification questions

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Rising Star
Hey guys,

I have about a gram of crude orange DMT leftover from an extraction that I am beginning to suspect may be contaminated with lye. The smoke is numbing to the lips and is extremely harsh. Additionally, several people have felt that they may have burned themselves smoking it due to "pull through" from the crystals. Admittedly, I did use an obscene amount of lye for a relatively small extraction. This all seems pretty characteristic of lye contamination. Don't worry, we're not smoking any more of it before it's cleaned up!

Anyway, I plan to recrystallize the stuff by dissolving it in some naphtha heated in a tall shot glass in a crockpot filled partially with water and then slowly cooling it with a seed crystal thrown in. However, I'm still worried about lye contamination as it seems that there's nowhere else for the lye to go but the final product? Should I dissolve the crystals in water first (possibly with a little bit of baking soda or something to ensure the pH is low enough and all of the DMT is in its freebase form) and then do a few naphtha pulls on it to separate it from the nasty lye? Then I could go on to recrystallize. Also, should the naphtha be hot at this point?

Also, what is everyone's opinion on using activated charcoal for dealing with discoloration issues during recrystallization? Is it worth it?
mrjefferson said:
Hey guys,
Should I dissolve the crystals in water first (possibly with a little bit of baking soda or something to ensure the pH is low enough and all of the DMT is in its freebase form) and then do a few naphtha pulls on it to separate it from the nasty lye? Then I could go on to recrystallize. Also, should the naphtha be hot at this point?

You're thinking along the right lines. First prepare a dilute solution of baking soda (pH~8.5). Then dissolve your spice into naphtha and do a couple of polar washes with your soda water. The water will take up the lye readily (lye is polar and doesn't like being in naphtha) without stealing any of your spice. Then you just reduce the naphtha to an appropriate volume and precipitate.

(See the Information subforum for a fairly complete discussion of the available purification techniques)
What constitutes a "dilute solution"? I don't have access to a pH meter or papers at the moment and I have really bad luck guessing at how much base to dissolve in solution - shit, that's what got me into this mess in the first place!

So the DMT will be lye-free and safe to smoke after this process? Is there any need to continue to recrystallize?
A dilute solution is constituted by pH ~8.5, as I said.

Get some damn pH papers ya lazy bum.

Yes, this process should get rid of all lye... depending on what else is in there, an activated charcoal treatment could be helpful... I wouldn't expect you'd need to recrystallize again though, as this is basically a recrystallization with an extra wash step.
Interesting - but I have never seen swim have to wash or improve her product except once, when she recrystallized. But 'orange' again, and from what tek..?.. oh let me ask -- ! Because we all Love to live and learn together ... What tek did you improvise on here - A-B or STB..@!?

For one 'rough' kitchen-science example SWIM has shown me, you can make a stock solution of dissolved lye that is Ph 14 by mixing 5 full teaspoons of Lye into 250 ml of hot water - this is a scortcher solution ! Screaming hot in alkalinity, and let it cool before using to basify... At 22 deg C it's at full scale on her pH pen ! Pulp mill pH !

Then (if you acidified to as low as pH 2.0 when doing a proper Acid-base separation), using less than 25 ml of the pH 14 solution, you will make the pH jump to 11.5 ! JUST 25 ml of the pH 14 stuff is enough to basify - watch it turn black at 20 ml ! If you acidified to pH 4.0 it'll be about 15 ml of the lye-stock solution to turn it black !! Hardly ANY lye at all to basify and 'chase' the dmt in to the naphtha !

... Any use of lye that goes into the 'excessive' is libable to backfire ... And YES !into the NP--solvent even ! A_B Teks that basify past 11.5 are being excessive with lye, and you'll also have to 'wash' the yeild, and lose product each 'wash'.

Hey everybody ... I love you all so much !... so I ask for safety and good-Hyperspace-trips' sake, ... Why bother being so 'sloppy' or rushed as to make a contaminated product ... !?

Please ask and read and learn, and don't take any steps for granted in any tek you try. pH Matters and it's easy to learn - borrow a pH meter just once and learn how many teaspoons of Lye it takes !! It'll really be like kitchen science and cooking with lye then ! My motto about lye use is "to taste is to waste " ... lye and spice !
Quoting wikipedia on lye:

"It is insoluble in ether and other non-polar solvents"

That being said, if one is extremely careful with the removal of the np, then one will get no lye out of it. If one transfers the np into a jar through a coffee filter, then one can see the traces of the brown lye contaminated solution get caught in the filter. the thickness of the lye/bark stew doesnt let it through the filter for the most part. if any does get through, one can transfer the contaminated lye/bark stew through another coffee filter. typically the contamination stays at the bottom of the first jar, but any that doesn't stick to the old jar will get caught in the coffee filter. this process can be repeated if one is sloppy until the remaining np is completely clear (with a possibility of a yellow tint from plant oils/trace amounts of red spice?). coffee filters are ones best friend.
Mitch - funny having to filter the NP solvent - it should be clear, with all emulsions settled, the NP solvent is clear no? If not let it settle and get a new turkey baster..?!

Lye is a hazard - don't assume it's 'stuck' somewhere, or what do you mean!? Who knows what the black slime is, or if lye is a visible contaminant, but that sounds like a real pulp-making-process if it's chunky in your filter !.

And let's not get confused by the the Wiki ref' re solubility of lye - it means that if you try to take lye pellets and drop them in Naphtha (ether), they will not dissolve at all. Naphtha cannot separate the ions of Na+ and OH- like water can in an instant.

But if you are talking about a water + lye solution mixed up next to a bunch of naphtha, something different happens, chemically speaking. NaOH (lye) ionizes in water, and these ions (Na+ and OH-) are even less attracted to the naphtha. So how does lye end up in naphtha, swim has asked me, when her yeild was gaghk !..?

I think this is because all chemical reactions always are also happening in reverse - to some degree ions of Na+ will meet up again with ions of OH- floating in the water and momentarily they become a single molecule of uncharged NaOH, which is able to 'live' in naphtha - where it will go if near naphtha !

Usually water re-separates the Na and OH again, but comparing a pH of 13 to 11 - in water, per second or minute it is 100 times more likely that NaOH forms at pH 13 than pH 11 - each pH point is a factor of ten times the concentration of OH- ...

So a dusting of NaOH molecules will seep into the naphtha from any watery solution of lye - the stronger the Lye solution, the more 'dusting' of NaOH molecules seep into the NP-solvent. This is different than lye-pellets dropped straight into naphtha.

And to prove lye contamination happens, it seems to swim that if you heat up a basified solution of MHRB, you get more NaOH contaminants in the naphtha. So even mishandling a pH 11.5 basified Non-Polar-extraction, you need to wash the yeild, just as with an STB pH of 13.5 or 'more'.
by the same token, if one was to use hcl for a/b, then there will be h+ and cl- in the mixture as well, thus leading to the possibility of extracting NaCl and hydrochloric acid, as well as lye (you're still adding lye to basify, no?) One is under the impression that none of these components are a result of any careful preparation.

and yes, the naptha layer is always perfectly clear (sometimes yellow tinted, but still clear). the separation technique can lead to the collection of small amounts of the black liquid (lye contaminated), but coffee filters, and further separation remove this.
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