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Re-x -- Recrystallization Pictorial Options
 
Hupecat
#1 Posted : 12/28/2019 9:13:47 PM
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Hello. I decided to share my way of re-xing with the community. It might be that if your spice is very impure, you need to give it a second run, but usually one run should be enough to result in clear white-spice. But its also possible with this way to result in clear see-through shards. In this Tutorial Heptane was used, but you could also use Naphtha. Hope its useful to some of you.


1. Weight out your amount of DMT that you want to re-chrystallize. (In my case its 1gr combined of 2 different batches, (pinkish and yellow-pinkish)






2. Prepare a waterbath on the stove, or crockpot. Put some Heptane/Naphtha in a non-sealed jar and keep it in the waterbath till near boiling, Have some cloth on the ground of the Cookpot, so your jar wont touch the ground of it.Small bubbles will appear on the sides of the jar. Be aware of the pressure building up in the jar and release it from time to time.






3. Put the DMT into the shotglass






4. Add the heated Heptane with an eyedropper to the glass with the DMT, as long as it looks all has been dissolved. U need to use just enough solvent to dissolve the spice. (I use a little Dabbing-stick to mix it thoroughly. There will be an orange blob on the bottom of the glass, and the Heptane turns slightly yellow.








5. Transfer with the eyedropper your Naphtha to another shot glass.. It will turn immediately cloudy, once it touches the new glass.be aware not to get any of the orange sludge with it.





6. Add just a few ml of clean hot Heptane to the first shot glass and mix again. Wait for settling and Then transfer it as well to the second glass, to get the rest of spice left, out of the orange goop.






7. Put the glass with the milky naphtha back into the warm bath. You already can notice another orange blob on the bottom of the glass. Keep it covered in bath for 30 min, and it becomes clear again. Have some cloth in the pot, so your glass won't touch the bottom of your pot.






8. Take it out of the heatbath. The Heptane has cleared again and on the ground you notice this orange goo blob.






9. Transfer the heptane once again to a new shotglass. It will turn milky immediately again touching the new glass. Fill bit clean heptane in glass 1 again and mix it.. transfer this also to the new glass, and do it another time with little Heptane.






10. Now Siphon all the heptane to your freeze-precip container (i used a shotglass as well here). And cover it with some foil.






11. Let it stand at room temperature for about 2-3 hours. You will notice some orange impurities at the bottom again, but i decided to leave it this time, as its not very much.






12. Then put in fridge for about 3-4 hours, and after that into the freezer for at least 12 hours.






13. Pour off the solvent and let the glass dry in front of a fan for about 10 to 15 min. (depends on the amount of Spice you recrystallize. You should have a glass full of nice white chrystals here.






14. Scrape them out of the glass, collect and enjoy. Swim should have transfered the heptane one more time to another shotglass. Now there still shows some yellow from the bottom of the glass.. But finally he ended up with 704mg nice sparkling off-white shards of DMT. Perfectly for e-mesh vaping.






I hope this Pictorial is easy to understand and of help for somebody. If you have any question about this, feel free to pm me.

 

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benzyme
#2 Posted : 12/28/2019 9:43:37 PM

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cool, but as a reminder.. yellow/orange spice may not necessarily be impure, just slightly oxidized. Most tryptamines turn yellowish with exposure to air.

I've had batches of syn spice turn from white to slightly yellow overnight. HPLC/MS spectra/chromatograms showed the same peaks.

what recrystallization is useful for is resolving oiled out product (which is generally just a supersaturated solution of dmt and impurities).
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benzyme
#3 Posted : 12/28/2019 9:50:12 PM

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Quote:
All crystallizations are based on the same principle: a solid compound
is fully dissolved in a solvent (or solvents) at a particular temperature,
the conditions of the solution are changed such that the solution becomes
supersaturated in the compound to be crystallized, and the compound
then crystallizes from the solution. Many compounds can crystallize in
more than one polymorphic form. For example, snow and hail are different
polymorphs of ice. The polymorph you get depends on the conditions
under which the crystallization takes place. Polymorphs have different
melting points and stabilities, so if you have difficulty in obtaining good
crystals from one crystallization system it is worth trying other systems.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
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ETH 0xd433198cb786145767c67d874b36cd7d42baf57a
 
Hupecat
#4 Posted : 12/28/2019 9:55:30 PM
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Yeah, thx.
As Swim still ends up with quite yellow product after a mini a/b, he prefers the old-school re-x.
I know, you have it explained already, but i do not find a solution for white chrystals after mini a/b..
 
benzyme
#5 Posted : 12/28/2019 9:59:28 PM

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I definitely know old-school, that's how I roll...DCM to extract, hexanes to re-x.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
XMR 46JqfBqi7JNM1W5rXXZ1FF1CBKKLoGEVBRya9Cn3RJmPbQhT4GeZpVKWbwaVe4vUMveKAzAiA4j8xgUi29TpKXpm3whx5MW
BTC 3CNrz6Tj17U35GLkRB1zsNtVoedorw8oja
ETH 0xd433198cb786145767c67d874b36cd7d42baf57a
 
 
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