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Recrystalization on STB Yield

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kagenical

Rising Star
I know this guy that yielded 1.4g of off white-yellowish spice from 110g of MHRB. This guy recrystallized once, and a thick, sticky yellow oil clung to the bottom of the beaker he used to recrystallize. It wasn't runny, and it didn't pool. It was glued in place.

Now, the clear portion of the solution from the recrystallization (although, it wasn't clear, but a transparent yellow) was freeze precipitated, the resultant DMT was collected and weighed in at 1.1g.


The only problem, however, is that this DMT, even after recrystallization, was still quite yellow. It's nowhere near the yellow of the first extraction (which looked almost like corn meal!) but it's still an offwhite, beige powder.

Is there anything he can do to get pure white crystals? He's tried to recrystallize again, but no pool of yellow gunk develops.

He thanks everyone.
 
I'm having a similar issue. I tried a recrystallization but no oily layer formed in the naphtha. Upon freezing, a thin yellow/orange layer formed at the bottom of the glass below the rest of the crystals which were pure white. I don't think there's much that can be done - it's probably some oil or fat that is slightly soluble in naphtha and that precipitates at about the same temperature range as DMT, which makes it difficult to separate. Perhaps there's another cleaning process that would help purify the crystals further (ammonia wash?).

One thing: be sure to limit the exposure of the drying crystals to air. When I first took the crystals out of the freezer they were pure white, but after 24 hours of drying they turned yellow at the edges. This indicates formation of DMT N-Oxide which is still psychoactive but less desirable than pure N,N-DMT. Using a fan or heat to dry the crystals will accelerate the oxidation process. Store the crystals in an airtight glass/metal container away from heat.
 
SWIM finds the best method to remove yellow by recrystallizing is to siphon off the spice rich liquid out of the shot glass and decant it into something else that you want to put into the freezer. This way favors the cleaner spice from the top rather than heavy yellow lye impurities you would get by vacuuming the bottom of the shot glass with your eyedropper.
 
SWIM is having the same problem.

Basically he's been looking around the site, reading up on the theory of recrystalization and although he has performed freeze percipitations himself before, he cannot understand how exactly its supposed to work. This is day 2 of research and he still can't understand it. Perhaps its just one of those mental gap moments, but he's done a bit of university chemistry and had problems understanding recrystalization then, too. He thought he was past that... But anyway:

If SWIM hypothetically takes 2.36g of yellow/tan waxy spice and dissolves it in a minimum amount of hot naptha.... as it says... the DMT was melting by this point of its own accord - so how can he tell the *minimum* amount of naptha?

and also, in a recrystalization, are the lipid impurities supposed to stay in the naptha? because they seem to be percipitating out, as well. either that, or it was just the melted (impure) dmt which then cooled down.

help plz!
 
its about 25ml naphtha per g of spice, so 59ml (lets say 60) ml in SWIYs case

dmt crystalizes once it cannot stay in a solvent anymore (due to too little solvent in evaporation or too cold solvent which makes it have smaller capacity to dissolve).

so thats it basically.. letting this warm naphtha (not too hot, you dont want dmt to vaporize away) for a couple of minutes, moving the container a bit, and it will dissolve the dmt and leave a layer of dark goo on the bottom.. This is impurities which do not redissolve in the naphtha because there is not enough of it, but the dmt will.. So just pippete the clear naphtha from the top and leave the goo behind. Then onto the fridge, which makes dmt crystalize purer than before.
 
Everything I have read points to recrystallization being something that you simply have to do a number of times before you get remotely 'good' at it. There are many different techniques such as using a pipette to pull the oil from the bottom of the vessel holding the dissolved spice, or the opposite - decanting the "more clear" liquid and leaving behind the junk. Part of this art, so I have read, involves knowing what to bring into the new spice and what to leave out. Since spice recrystallizers are often working on small quantities they seem loathe to let hardly anything "slip away". Of course, one could collect the goo and use it on leaf or something else...

This one appears to be a live and learn technique. Just save all 'gunk' and freeze precip from the solvent. One can always try to clean up the gunk if they are interested.. Like anything one is learning, it is generally not a good idea to "try out" some new technique with all of your valuables. Inch it along..


So I am told...

{h}
 
Mmnmn.. thankyou for the replies. SWIM has done this before in the past, successfully, but lately he forgot how to do it (Because its been a while since he did it last.)
 
Fatcat said:
How hot would be too hot? would heating up the shot glass with a blow dryer for 5 min, or so, work?
Click to expand...

dont know what temperatures the blow dryer reaches. Too hot = 60 or more degrees celcius. This could vaporize at least some of the dmt away.

SWIM knows that around 40-50 degrees celcius is when the water starts getting too hot to touch. So SWIM heats up water to this point where it just gets too hot to touch, turns the fire off, puts the solvent in a glass which already has the dmt in it, submerges the glass in the warm water (without letting the water come in the glass of course), leaves for a min or so, moving the glass in circles to make a movement of the solvent and help redissolving.

halcyon said:
Everything I have read points to recrystallization being something that you simply have to do a number of times before you get remotely 'good' at it. There are many different techniques such as using a pipette to pull the oil from the bottom of the vessel holding the dissolved spice, or the opposite - decanting the "more clear" liquid and leaving behind the junk. Part of this art, so I have read, involves knowing what to bring into the new spice and what to leave out. Since spice recrystallizers are often working on small quantities they seem loathe to let hardly anything "slip away". Of course, one could collect the goo and use it on leaf or something else...

This one appears to be a live and learn technique. Just save all 'gunk' and freeze precip from the solvent. One can always try to clean up the gunk if they are interested.. Like anything one is learning, it is generally not a good idea to "try out" some new technique with all of your valuables. Inch it along..


So I am told...

{h}
Click to expand...

SWIM would never ever keep the gunk. What he does is add another, say, 5ml of warm naphtha to pick up any last rests of dmt that might be in the gunk, but he definitely throws it away after that.
 
Totally out of curiosity, I took my freezing naptha out of the freezer to check on it, and I noticed that when I breathe on it, little white lines form on the surface. Is that precipitating DMT?
 
Fatcat said:
Totally out of curiosity, I took my freezing naptha out of the freezer to check on it, and I noticed that when I breathe on it, little white lines form on the surface. Is that precipitating DMT?
Click to expand...
No, it's probably ice from the water vapor in your breath.

Another reason the naphta should not be too hot is the danger of 'oiling out'. This happens when at cooling down, droplets of DMT are formed instead of solid crystals. This liquid DMT traps contaminations, so keep it below the melting point of DMT, say 40 C.
I think the boiling point of DMT is much higher than people often assume.. I tried to evaporate it at 100 C (boiling water) but it just melts, no evaporation at all. And yes, I'm sure it was freebase DMT!

Defatting can help:
- dissolve the impure spice in dilute HCl
- filter if there is solid crap in it
- wash a few times with toluene or DCM to defat
- basify, watch the whitish DMT precipitate
- pull with naphta and freeze precipitate as usual
 
SWIM had a simmilar problem develop but not until its 3rd re-cryis using the same container, I can only assume that it was the unwashed junk/sludge it had left on the bottom of the glass contaminating the color of the product, SWIMS first two trys produced nice white spice, since then it always comes out a pale yellow. Swim also suspects his solvent was an issue as he was trying to reuse the same re-crysisng solvent (Naptha) over and over again.

SWIM plans on being more methodical about his tool cleaning in between pulls from now on but would still like to reuse the solvent.

Starting a new batch, SWIM will be spending allot of time on purification methods this time around as SWIM will have more then enough spice to toy around with properly.
 
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