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Growing spice xtals


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#21 coorsmikey

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Posted 20 December 2017 - 09:50 AM

Ok while we have you around I don’t mind asking away! So I have been freeze precipitating to get the xtals. Then I take the same solvent from the FP and it goes back into my Basic solution to see if I can get more or all the DMT out. Each time it does appear that I am getting more back as when I freeze precip it again I am getting more Xtal. What’s wrong with doing it that way, or should I be using fresh solvent to get maximum absorption from the Basic Solution?

Another question. I have been able to separate the white Xtal in the FP but in the final evap I get nice “mini xtals” that I can scrape out the individual clusters and have a nice crystalline stash, but I still get a sticky goo that is almost invisible in the evap dish. When scraped up it an orange goo that sticks to anything I handle it with. The goo is very temperature sensitive, at any temp above room temp it will turn to a liquid mess. The goo is definitely active but not so great for storage. Does Freddy have an idea on how to turn that goo to Xtal? I don’t even care if it stays orange really?

Edited by coorsmikey, 20 December 2017 - 09:51 AM.

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#22 Phineas_Carmichael

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Posted 20 December 2017 - 07:11 PM

Ok while we have you around I don’t mind asking away! So I have been freeze precipitating to get the xtals. Then I take the same solvent from the FP and it goes back into my Basic solution to see if I can get more or all the DMT out. Each time it does appear that I am getting more back as when I freeze precip it again I am getting more Xtal. What’s wrong with doing it that way, or should I be using fresh solvent to get maximum absorption from the Basic Solution?
...

Nothing is wrong with freezing and reusing solvent for the next pull on the basic solution.  In fact, it is how things should be done IMO.  When you freeze all the crystals out your solvent is basically "empty" and you can use it again.  Using fresh solvent for every pull would be wasteful, expensive, and ecologically irresponsible.  Let's face it, most clandestine chemists don't dispose of their solvents properly.
 
I work in QC at a facility where we use a lot of different solvents and chemicals, and we are very concerned about our "waste streams."  Gone are the days of just dumping it in the river (in fact, that river caught on fire some years ago so we don't do that anymore...) and now we save our waste in big drums.  What waste we can safely burn we incinerate on site to generate electricity for the facility, other waste goes to hazmat disposal companies where they do the same thing with a more sophisticated incinerator.
 
I would love to see clandestine chemists (and painters, and backyard mechanics) take their used solvents and such to local hazmat collection sites whenever possible.  Sadly, I think most just throw old chems in the trash or evaporate them and they end up "in the river" anyway.
 
*rant over*
 
Mikey, since you are freezing out each pull from the basic solution and reusing the solvent, I would be very curious to see yield data from each pull.  Logic says the first pull will grab most of the DMT, subsequent pulls grabbing less and less each time, but I've never seen data on that and Freddy never even thought to do it that way.  If we knew that the first pull got 100mg, the 3rd got only 6mg, and a 4th got nothing, we would know that 3 pulls is actually the ideal number...  Feel like doing a project? 

...
Another question. I have been able to separate the white Xtal in the FP but in the final evap I get nice “mini xtals” that I can scrape out the individual clusters and have a nice crystalline stash, but I still get a sticky goo that is almost invisible in the evap dish. When scraped up it an orange goo that sticks to anything I handle it with. The goo is very temperature sensitive, at any temp above room temp it will turn to a liquid mess. The goo is definitely active but not so great for storage. Does Freddy have an idea on how to turn that goo to Xtal? I don’t even care if it stays orange really?

The orange goo!!!

 

We used to call it "The Haitian Shit" because of that shitty Jason Statham movie...

DSyCzuDbMwc

 

Does that vial of goo on the right look familiar?

 

3 Vials.jpg

 

It is very definitely active, and is definitely a mess to store and work with, but over the long term (my buddy Prichard Evans is a psychedelic camel and kept a vial in his "head stash" for several years) it does solidify into a kind of paste (like bong resin) instead of a liquid.  My hypothesis is that the Haitian Shit is a mixture of alkaloids, perhaps chiefly yuremamine, with some other DMT derivatives and a small amount of N,N-DMT that didn't get completely frozen out.

 

You could conceivably recrystallize the N,N-DMT by dissolving the goo in hot solvent, then cooling slowly until the goo settles to the bottom of the beaker and decanting the solvent off, evaporating it until it gets cloudy and freezing.  But you'd still be left with the goo...

 

I don't know how to crystallize the goo into "jungle spice" without years of storage though.  Perhaps gentle heat with stirring over time would solidify it in less time?  In PiHKAL, Dr. Shulgin talks about leaving things on a stir plate in his lab for weeks & months just to see what happens, I think this goo would be a perfect candidate for this kind of treatment...

 

Sorry I couldn't be of more help.


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#23 coorsmikey

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Posted 20 December 2017 - 07:53 PM

Yours and Freddy’s input is most valued and appreciated! Always has been.

Yes the good is exactly as you described and I also get the same results with time, it does end up thickening up and am able to handle.
I am willing to pass on some info to Freddy as far as the results of first second and third pull. I can have my buddy do a 100gr of bark to keep the numbers simple and easy to grasp. I may even post my buddy’s method due to the simplicity of the tek and others can chime in and compare the results to some of the more complicated time consuming tek I see being use so often. I might have to wait til after the new year to actually post the results for the multiple pulls.

Thank you for the confirmation on the opinion of the solvent being pretty much “empty” after the DMT has crashed. Also I do feel that it is important be as ecological responsible as possible. I don’t think we can talk about that enough, and it is great to have Phineas_Carmichael reiterate the concept.
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#24 Soliver

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Posted 20 December 2017 - 09:31 PM

Man, I have got to come back to this thread over the xmas break and do some serious reading / thinking / studying / re-reading ...

 

I don't even know the questions I need to ask, but this sounds ... like fun. 

 

Thanks to all for sharing the knowledge - I've got some research ahead of me.

 

:)

 

soliver


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#25 Phineas_Carmichael

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Posted 21 December 2017 - 02:41 AM

 

That, my friends, is some excellent advice. Archive Material

 

 

...
P. Carmichael you know what your talking about.

 

Yours and Freddy’s input is most valued and appreciated! Always has been.

 

...

Thank you for the confirmation on the opinion of the solvent being pretty much “empty” after the DMT has crashed. Also I do feel that it is important be as ecological responsible as possible. I don’t think we can talk about that enough, and it is great to have Phineas_Carmichael reiterate the concept.

Ya'll keep talking like I'm some kind of "spice jedi" and, while I appreciate the compliments, it kind of makes me uncomfortable...

 

Like Zaphod Beeblebrox, I'm "just zis guy, you know?"  I may speak with authority, but I stand on the shoulders of Giants like Norman, Director of Sound, Waylitjim, Tregar, Phlux, and many others.  It just so happens that I was studying chemistry in University when my buddy Freddy got interested in clandestine chemistry & I was able to  help him apply the techniques from the O-chem lab to his experiments on his sloop in International Waters...

 

Right time, right place, ya dig?

 

...
I am willing to pass on some info to Freddy as far as the results of first second and third pull. I can have my buddy do a 100gr of bark to keep the numbers simple and easy to grasp. 

...

I might have to wait til after the new year to actually post the results for the multiple pulls.

...

Take your time.  I hate to give you "homework," but I am mighty curious to see an extraction with controlled numbers; I have a weird data-boner...

 

Sadly, Freddy and I can't play around like we used to so we have to live vicariously through you folks...

...

I may even post my buddy’s method due to the simplicity of the tek and others can chime in and compare the results to some of the more complicated time consuming tek I see being use so often.

...

DO IT!

 

Mycotopia has a wealth of "grow logs" for marijuana and mushrooms, but there are precious few "extraction logs" and that makes me sad.  For some reason people don't feel the need to post their extractions step by step with pics like they do their other projects.  Maybe it's because an extraction can be "quick-and-dirty" following a "TEK" and finished in a few days while a mushroom grow takes 100 days?  Whatever the reason I have always thought that we should be documenting our extractions without thinking that we are posting a new TEK.

 

I, for one, would love to see your buddy's simple method.

 

"Daddy loves a Mason Jar"  --  Allow me to toot my own horn and shamelessly self-link for a minute, but the A/B vs STB Side By Side thread was one of Freddy's first experiments and made extensive use of mason jars and baking dishes...

Man, I have got to come back to this thread over the xmas break and do some serious reading / thinking / studying / re-reading ...

 

I don't even know the questions I need to ask, but this sounds ... like fun. 

 

Thanks to all for sharing the knowledge - I've got some research ahead of me.

 

:)

 

soliver

 

There is nothing like the fun to be had in "the lab," whether your lab is a temporary one on the kitchen counters or in the bathtub or a dedicated space in the walk-in closet.

 

There is great joy to be found in turning a pile of plant stuff into a pile of "brain candy." -- Sooooo satisfying.

 

Far more satisfying when you're bored than buying a pack of cigarettes...

 

;)

 

Phin


Edited by Phineas_Carmichael, 21 December 2017 - 02:48 AM.

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#26 invisibilitysyndrome

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Posted 21 December 2017 - 10:51 PM

Hey all
So I did peruse the ab and stb side by side. Deff a very cool comparison. Probly do a/b on the next go around. usually Always do stb and get 1.7%. not as good as the a/b in the comparison but not bad.

So I happen to have some notes on a stb done on 10 oz (280g ) purple brazillian inner root bark strips.
Done in one gallon of h2o. 280 g lye 250mills naptha
Pulls werent phenomenal at 1g and .5 g 2nd pull
However 100 g salt was added after 2nd pull and it yielded 1.2 g 3rd pull and fairly clean white to boot
Stopped taking notes after 3rd pull.
I spose had I continued to keep records id have known when the pulls become superfluous

I would also like to add that doing a re x will deff for sure yield nice solid xtals when solvent is left to evaporate.
Dont have notes and the pics are un available from previous rex but by placing desired amount of clean product free of any oils in smallest amount of solvent that will absolutly disolve all D when warm or even hot.

Solvent being heptane or even naptna
Leave this to evaporate like was stated above and it will grow beautiful solid xtals more D the bigger and better the xtals.
The key as stated is slow as possible with no air movement or dust. Over thecourse of a few days of no touching it will begin to grow.

Doing a slow cool and crashing the D out of solvent will yield snow no matter what it will however yield a cleaner end result reducing the need for future clean up.

A note on evaporating the solvent. IME letting the solvent evap after all the work is done will yield any thing left behind. Most often orange goodand a small amnt of D. So depending what the desired final end result is evaporating will still yield something however minute.

Some one also mentioned the Orangegoo and how to make it solid.
Id say the best way is to just add some D to it and it will mix together and be ez to store handle and use.
It will be a bit more harsh but it is better than the clean white Imo.
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#27 Cigarsam

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Posted 24 December 2017 - 08:05 AM

Gotta say good info headed this way. Taking notes.
Friend noticed a huge different in the quality of white to yellow to even a brown sugar looking xtals by just doing a fertilizing his brown goo.
Left in freezer for a good 48 hours. Only small white (once) and yellow xtals. After the cleaning of the brown goo using only naphta it turned into some quality brown looking sugar.
Only using Cybs hybrid salt tek STB.
Small batches and hasn't found a good way to break the fibrous R.B. down in order to use his 1000ml seperatory funnel.
Just ordered a metal grinder with hopes of sharpening up his blades for better chopping of the shredded M.H.R.B.
Can't use his funnel at the moment due to the stopper getting chocked up.

Edited by Cigarsam, 24 December 2017 - 08:06 AM.

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#28 Cigarsam

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Posted 27 December 2017 - 06:29 PM

That would be a clean up of the brown goo ( re-crystallization) produced some excellent brown like sugar.∆∆
A Dremel metal grinder works well for sharpening the blades for the blender to produce more powder too.
This turning out to be interesting thread.
Looking forward to any "teks" posted here.
Peace

#29 Heirloom

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Posted 27 December 2017 - 08:58 PM

invisilibitysyndrome or anyone just how big can D xtals get? I don't have much experience, never got goo, just white snow and some yellow. I enjoyed doing it but it scares the hell out of me, still trying to apply what I learned from the few experiences I had. Can't say if I'll every try it again. Like most here I'm fascinated by psycho actives.

Anybody ever dye anything?
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#30 Phineas_Carmichael

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Posted 30 December 2017 - 03:19 AM

...
Only using Cybs hybrid salt tek STB.
Small batches and hasn't found a good way to break the fibrous R.B. down in order to use his 1000ml seperatory funnel.
Just ordered a metal grinder with hopes of sharpening up his blades for better chopping of the shredded M.H.R.B.
Can't use his funnel at the moment due to the stopper getting chocked up.

Unfortunately, in my buddy Freddy's experience no matter how fine you powder the bark you'll never be able to use a sep funnel to separate an STB pull.  By the time the solvent settles out, the fine particulate will have made a solid mass in the bottom of the funnel & clogged the stem.  The hole in the stopcock is just too small.  Sorry.

 

However, you could conceivably use a gravy separator, provided it was large enough and made of pyrex or another lye & solvent safe material:

img88o.jpg

This one holds at least 1L and is from "Willems-Sanama" (intentional misspelling so Topia doesn't accidentally show up in Google searches for my favorite cookware company)

 

invisilibitysyndrome or anyone just how big can D xtals get?

...

Well, there's that spectacular picture on Erowid from an "Anonymous Photographer"

dmt_crystal1.jpg

If the photographer is to be believed, this one is ~1 inch wide

...

I enjoyed doing it but it scares the hell out of me, still trying to apply what I learned from the few experiences I had. Can't say if I'll every try it again.

...

You and me both, brother.  I have very little desire to do it again, but I sure love facilitating the experience for others!


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#31 Rudeboysteven

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Posted 30 December 2017 - 01:16 PM

I was thinking about this at work today and a few things occurred to me...

...
I have a vac purge with a recovery pump. And I recently did it with heptane and got the prettiest mini xtals I've ever seen. Accept when they are scrapped they turn to fine xtal dust. Not very appealing or even stable . too much surface area exposed to oxidize.
...


Do I understand correctly that you have a device that lowers the BP of your solvent with vacuum and recovers the solvent? Like a rotary evaporator? If so, badass and quite ecologically responsible. : The reason you're not seeing large crystals is, again, time. When you boil off all the solvent (at low temperature because of the vacuum) there simply isn't enough time to build large crystals.

Let's play a game:
Imagine your solvent as a circle in a parking lot, and your DMT as a bunch of people inside that circle. The object of the game is to make sure that everyone stays inside the circle as long as possible, and if a person steps out of the circle they have to go down on their hands & knees. It's basically "The floor is lava" outside the circle and everyone wants to help everyone else stay inside.

When you start to evaporate (or cool in the case of freeze precipitation as above) the solvent the circle starts to shrink and the people get closer and closer together until they can't all fit on the circle anymore and some are forced to crouch on their hands & knees. If the circle shrinks quickly, you just end up a bunch of people on their hands and knees... Small crystals.

But, if you shrink the circle slowly, a few people drop to their hands and knees and that makes more space for the rest of the people because they can climb on top of the ones on the ground. Then, as the circle gets smaller, the people start to cooperate and climb on top of the people on their hands and knees and make a human pyramid to make more space for everyone else in the circle. The slower you shrink the circle, the more time the people have to make a pyramid... Big crystals.

Take it one step further and add your seed crystals to the equation. This makes it so the game starts with some people already on their hands & knees, the building blocks for human pyramids are there right from the beginning! Some of the people will choose to go on their hands and knees next to the seed crystals to give everyone else more time as the circle shrinks and they will be able to make a bigger pyramid. You have to give your people as much time to cooperate and make human pyramids as possible, because that shit is hard!

Does that make sense to anyone but me? :weedpoke:

...
I want shards . of spice. And like. I can't do it in the air too much dust and air contam . pls help

This got me thinking. The biggest and best crystals are made by very slow evaporation of the solvent. I remember Phlux or Director of Sound talking about a bucket of harmala alkaloid solution that he forgot in the shed for a couple of months and discovered giant crystals when he found it again. Obviously you can't evap in open air because of dust, like you said. But...

BUT.......

What if you made a supersaturated solution as described above, let it cool until it started to get cloudy & seeded it with a pure crystal, then covered the container with a porous fabric? Something that wouldn't let dust in, but would let solvent vapor out, like a thin T-shirt or maybe even TyVek. I bet you could grow some gnarly shards if you let it sit for a week or two (or more?) and slowly evaporate that way...
Blown away

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#32 Rudeboysteven

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Posted 30 December 2017 - 01:20 PM

Ok while we have you around I don’t mind asking away! So I have been freeze precipitating to get the xtals. Then I take the same solvent from the FP and it goes back into my Basic solution to see if I can get more or all the DMT out. Each time it does appear that I am getting more back as when I freeze precip it again I am getting more Xtal. What’s wrong with doing it that way, or should I be using fresh solvent to get maximum absorption from the Basic Solution?
...

Nothing is wrong with freezing and reusing solvent for the next pull on the basic solution. In fact, it is how things should be done IMO. When you freeze all the crystals out your solvent is basically "empty" and you can use it again. Using fresh solvent for every pull would be wasteful, expensive, and ecologically irresponsible. Let's face it, most clandestine chemists don't dispose of their solvents properly.

I work in QC at a facility where we use a lot of different solvents and chemicals, and we are very concerned about our "waste streams." Gone are the days of just dumping it in the river (in fact, that river caught on fire some years ago so we don't do that anymore...) and now we save our waste in big drums. What waste we can safely burn we incinerate on site to generate electricity for the facility, other waste goes to hazmat disposal companies where they do the same thing with a more sophisticated incinerator.

I would love to see clandestine chemists (and painters, and backyard mechanics) take their used solvents and such to local hazmat collection sites whenever possible. Sadly, I think most just throw old chems in the trash or evaporate them and they end up "in the river" anyway.

*rant over*

Mikey, since you are freezing out each pull from the basic solution and reusing the solvent, I would be very curious to see yield data from each pull. Logic says the first pull will grab most of the DMT, subsequent pulls grabbing less and less each time, but I've never seen data on that and Freddy never even thought to do it that way. If we knew that the first pull got 100mg, the 3rd got only 6mg, and a 4th got nothing, we would know that 3 pulls is actually the ideal number... Feel like doing a project?

...
Another question. I have been able to separate the white Xtal in the FP but in the final evap I get nice “mini xtals” that I can scrape out the individual clusters and have a nice crystalline stash, but I still get a sticky goo that is almost invisible in the evap dish. When scraped up it an orange goo that sticks to anything I handle it with. The goo is very temperature sensitive, at any temp above room temp it will turn to a liquid mess. The goo is definitely active but not so great for storage. Does Freddy have an idea on how to turn that goo to Xtal? I don’t even care if it stays orange really?

The orange goo!!!

We used to call it "The Haitian Shit" because of that shitty Jason Statham movie...
DSyCzuDbMwc

Does that vial of goo on the right look familiar?

attachicon.gif3 Vials.jpg

It is very definitely active, and is definitely a mess to store and work with, but over the long term (my buddy Prichard Evans is a psychedelic camel and kept a vial in his "head stash" for several years) it does solidify into a kind of paste (like bong resin) instead of a liquid. My hypothesis is that the Haitian Shit is a mixture of alkaloids, perhaps chiefly yuremamine, with some other DMT derivatives and a small amount of N,N-DMT that didn't get completely frozen out.

You could conceivably recrystallize the N,N-DMT by dissolving the goo in hot solvent, then cooling slowly until the goo settles to the bottom of the beaker and decanting the solvent off, evaporating it until it gets cloudy and freezing. But you'd still be left with the goo...

I don't know how to crystallize the goo into "jungle spice" without years of storage though. Perhaps gentle heat with stirring over time would solidify it in less time? In PiHKAL, Dr. Shulgin talks about leaving things on a stir plate in his lab for weeks & months just to see what happens, I think this goo would be a perfect candidate for this kind of treatment...

Sorry I couldn't be of more help.
Kill all de whitebman

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#33 Rudeboysteven

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Posted 30 December 2017 - 01:26 PM

Hey has anyone seen the new season of Hamilton's phamecopeia ? There's a dmt segment episode. Now from what I seen. They're basically glorifying dmt kitchen alchemy to the masses . encouraging it. And out in a while clip of how to frrlee base it on STB tek

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#34 Rudeboysteven

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Posted 30 December 2017 - 01:26 PM

Hey has anyone seen the new season of Hamilton's phamecopeia ? There's a dmt segment episode. Now from what I seen. They're basically glorifying dmt kitchen alchemy to the masses . encouraging it. And out in a while clip of how to frrlee base it on STB tek

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Scary

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#35 Rudeboysteven

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Posted 30 December 2017 - 01:26 PM

Hey has anyone seen the new season of Hamilton's phamecopeia ? There's a dmt segment episode. Now from what I seen. They're basically glorifying dmt kitchen alchemy to the masses . encouraging it. And out in a while clip of how to frrlee base it on STB tek

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Scary

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M. hostilis is gonna be banned soon

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#36 Rudeboysteven

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Posted 30 December 2017 - 01:32 PM

Thank you everyone for all your replies. Just getting back from holiday to come back to head fullz of reading/advice/new experiments. I hope I have time to reply to everyone as soon as possible. I am sad to say (and I am not putting the movement down in any way) But I would never get any kind of feedback on the NEXUS in the 3 years I have been there. It's like u have to be an entity of some import to get any where in the forum. Any ways I love the NEXUS but the feed back and positivity is crazy on here. Thank you and happy New year. Exctied to learn more this year.
Namaste

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#37 Defiance

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Posted 02 January 2018 - 06:54 AM

Phin ( :hug:) hinted at this in his first post, but my nicest crystals came from seeding liquid DMT freebase.

 

You can crash out liquid DMT by supercooling a saturated solution in a saline ice bath in the freezer. The freebase is cloudy white and will crystallize spontaneously if you even look at it wrong. Use extremely clean glassware and a steady hand. Watching shards form before your eyes because you jostled the flask is really cool, but it means you have to start over.

 

To get the solution and seed crystals, you need to clean up your regular pulls until there is little to no yellow/orange goo. I usually recrystallize with heptane, but you can also use chilled absolute isopropanol to selectively dissolve the goo and leave the crystals behind. 

 

Once you have clean shards, dissolve them in a minimum of barely warm naptha, and run slowly down through the temps as Phin outlined. I had better luck with naptha than heptane, it's just too hard to supercool a heptane solution, crystals precip and then grow much too fast. 

 

The solution of supercooled DMT and naptha will form layers, and you can carefully pipette off the crystal clear solvent from above the cloudy freebase. 

 

Once you've got supercoold DMT freebase in a flask with most of the solvent off, you need to slowly bring it up to room temperature then seed it and cross your fingers. Most of the time it spontaneously crystallized, but a few times I grew individual crystals ~300mg over the course of a day or two.

 

My guess is the really huge crystalline chunks you see on Erowid are the product of distillation, which needs to be carried out under an inert atmo with very careful temp control because the DMT will tend to clump and scorch in the distillation flask as you near dryness, probably using an oil substrate in the distillation flask is the answer but I never tried it. Inert atmo with vacuum and an extremely short column with hot water above DMT MP running through will mostly stop spontaneous crystallization in the joints. DMT distillation sucks. 

 

Anyway in my experience you really need liquid DMT to grow big chunky crystals, and the more of it you have laying around the better.


Edited by Defiance, 02 January 2018 - 06:56 AM.

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#38 Heirloom

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Posted 02 January 2018 - 08:12 PM

some xtals long ago vaporized

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#39 Phineas_Carmichael

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Posted 03 January 2018 - 01:35 PM

Phin (  :hug:) hinted at this in his first post, but my nicest crystals came from seeding liquid DMT freebase.

...

I thought I might draw you out with that if you were still around...  

 

So good to see you; thanks for helping me to stand on your Giant shoulders!   :hug:

 

...

My guess is the really huge crystalline chunks you see on Erowid are the product of distillation, which needs to be carried out under an inert atmo with very careful temp control because the DMT will tend to clump and scorch in the distillation flask as you near dryness, probably using an oil substrate in the distillation flask is the answer but I never tried it. Inert atmo with vacuum and an extremely short column with hot water above DMT MP running through will mostly stop spontaneous crystallization in the joints. DMT distillation sucks. 

 

Anyway in my experience you really need liquid DMT to grow big chunky crystals, and the more of it you have laying around the better.

:wub:


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