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Diazin
#21 Posted : 1/7/2017 9:49:39 PM
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By the way, this tek will only work for totally nps's I think for it to leave out pure white dmt, which to my knowledge there's none which will dissolve dmt at room temp. You might try heptane/hexane, but they would have to be warmed up prior to use. Also, there's some suspicious hexane might actually be carcinogenic...
 

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pitubo
#22 Posted : 1/7/2017 9:51:04 PM

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Diazin wrote:
Does dmt even freeze-precipitate from ethanol at home-freezer temp? I dont think so as dmt is very soluble in ethanol.

You can't because dmt is still very soluble in cold ethanol. It might be so that cooling supersaturated ethanol causes some of the dmt to crystallize out, that would still be an interesting approach to purify at least a part of an amount of dmt. My experience with crystallizing dmt from evaporating ethanol showed only goo dropping out from the start though, no nice crystals appeared at any part of the process.

Diazin wrote:
BUT, you could perhaps try this:

[..suggestion to mix brine and ethanolic dmt..]

It would not work. When you mix sodium chloride solution and ethanol, the ethanol instantly causes the salt to drop out of solution.
 
downwardsfromzero
#23 Posted : 1/7/2017 9:53:19 PM

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Feoom wrote:
Thank you anyway... I have recrystallized using heptane and it worked out okay. But it took a few days. Thats why i am very interested in the tek i am researching about, that doesn't use evaporation techniques.


Good crystallisation takes time. It's a fact of life. Why the hurry?



Ruining Beer wrote:
It's not what you said, it's the way you said it.


Considering pitubo's first language is not English, I'd say pitubo is doing a pretty good job... Nexus members need to be aware of the diversity of culture in the forum - this awareness helps one to avoid being upset by "somebody else's tone" Wink



Diazin wrote:
3 - Add saline water to the pasty spice, add alot of water, some 300ml or so for every 1ml of ethanol, and put it to freeze-precipitate


Adding ethanol to saturated saline will produce nice crystals... of sodium chloride. Aim for slightly below saturation if you're trying this.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
pitubo
#24 Posted : 1/7/2017 9:54:33 PM

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Diazin wrote:
Also, there's some suspicious hexane might actually be carcinogenic...

Surprise: Ethanol, or at least its inevitable metabolic product acetaldehyde, is a known carcinogen.

https://en.wikipedia.org/wiki/Alcohol_and_cancer
 
Diazin
#25 Posted : 1/7/2017 9:59:18 PM
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But in this case wouldnt the amount of crashed-out salt be minimal, perhaps not even visible? I mean, a 300:1 water/ethanol ratio is atrocious, the ethanol is there mostly to aid dmt releasing the gunks into the ionized water only...
 
Diazin
#26 Posted : 1/7/2017 10:03:57 PM
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pitubo wrote:
Diazin wrote:
Also, there's some suspicious hexane might actually be carcinogenic...

Surprise: Ethanol, or at least its inevitable metabolic product acetaldehyde, is a known carcinogen.

https://en.wikipedia.org/wiki/Alcohol_and_cancer


Ohh yeah, there's that....
 
pitubo
#27 Posted : 1/7/2017 10:05:53 PM

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downwardsfromzero wrote:
Ruining Beer wrote:
It's not what you said, it's the way you said it.


Considering pitubo's first language is not English, I'd say pitubo is doing a pretty good job... Nexus members need to be aware of the diversity of culture in the forum - this awareness helps one to avoid being upset by "somebody else's tone" Wink

While I will not dispute my less than perfect command of the English language in all its subtleties and idiosyncrasies, I don't believe that this was in fact the real cause of contention. I am under the firm impression that my (constructive) criticism of Running Bear's compositional style caused the complaints about my "tone". The further derailment into vapid attempts at insulting to me only confirm the very personal nature of Running Bear's subsequent contributions to the thread.

I'm confident that tomorrow, Running Bear will resent the lapse of better sense.
 
Feoom
#28 Posted : 1/7/2017 10:22:21 PM
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pitubo
#29 Posted : 1/7/2017 10:42:32 PM

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Feoom wrote:
So my next question is: When does Freebase DMT dissolve in water? When heated? Near Boiling point? Stirred? Combination of all?

All solubilities are subject to limits, though these limits may be affected by temperature. So, at room temperature, X grams of dmt would dissolve in 1 liter of water, while at the boiling point of water, the amount may be Y. Stirring does not change solubility, it only accelerates the dissolution, up to the set limit.

Only liquids that are miscible in any proportion, such as water and ethanol, have no such limit. But then again, in this case it is about mixing, not solubility. Many pairs of solvents (eg. water and hexane) also have an associated limit of solvability (or dissolution? please help me out with my english, downwardsfromzero Big grin ).
 
downwardsfromzero
#30 Posted : 1/7/2017 10:48:59 PM

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pitubo wrote:
solvability (or dissolution? please help me out with my english, downwardsfromzero

Er, how is this different from "solubility" which you used in the preceding sentence? I'm approaching my normal bedtime brain-failure point but mutual solubility is all I can come up with at the moment.


Feoom wrote:
If Freebase DMT is still soluble in ethanol at room temp the rek could work out. The only question is left how about water. I have read that Freebase DMT is undissolved in water but other thread and claims state that its almost undissolved in water.

So my next question is: When does Freebase DMT dissolve in water? When heated? Near Boiling point? Stirred? Combination of all?

The whole idea is heating up the solvents to boiling point with minimul amount of solvent. so when it cools down the DMT crashes out in form of crystals. thats why its so important that a solvent keep dmt undissolved and the other solvent keep dmt disolved so the one of the solvents crashes the DMT out in crystals because the solvent 1 and solvent 2 are mixed (100% miscibility)

Thinking back to my days of learning lab technique, we used aqueous ethanol for some org prep recrystallisations. When heated, less polar substances dissolve more into the EtOH (aq) and crystallise back out again on cooling. This may or may not be of use WRT DMT, and the appropriate alcohol dilution would have to be determined experimentally/experientially. When the data does not exist, you have to try it out for yourself.

Attempts at purification using aqueous IPA seem to lead to ever-increasing amounts of reddish gunk so I wouldn't hold my hopes out too much for aqueous ethanol either. I get the feeling lower alcohols promote the oxidation of DMT slightly, perhaps due to greater oxygen solubility.

(Reading back to p's warning about heating flammable solvents, we always heated our ethanol on the steam bath of course. And my support for p's criticism was worded in a particularly obscure manner, even for an "Englishman".)




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
pitubo
#31 Posted : 1/7/2017 11:04:06 PM

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downwardsfromzero wrote:
I get the feeling lower alcohols promote the oxidation of DMT slightly, perhaps due to greater oxygen solubility.

This was in fact my experience when experimenting with recrystallization from ethanol: white spice snowflakes turned into yellowish goo. It made fine changa nevertheless.

downwardsfromzero wrote:
And my support for p's criticism was worded in a particularly obscure manner, even for an "Englishman".)

If I were to attempt to recrystallize dmt from an English ale, would I ruin the dmt or would I be ruining the beer? Laughing
 
Mindlusion
#32 Posted : 1/7/2017 11:26:56 PM

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Feoom wrote:


The recrystallization method i am researching doesn't require freeze participation or evaporation. The reason why i ask if Freebase DMT is soluble in Ethanol in room temperature is because there is no single solvent (that i know off) i can use for my recrystallization method. ideally 1 solvent should be perfect. But i don't know any solvent that keeps Freebase DMT undissolved at room temperature but completely dissolves Freebase DMT near the boiling point.



Yes there is, use heptane.

You don't need a tek, just a basic understanding. Every case is different so a recipe won't do you any good.

You have right idea, use just enough solvent to completely dissolve it at boiling or near boiling. Then pour off the supernatant into a clean flask or container, leaving behind any residue that does not dissolve. Then slowly cool to room temperature, then fridge, and freezer if necessary. You should get crystals before going to the fridge. I usually just use the fridge or freezer to push out any last product.

Sometimes you do want slow evaporation, if your not getting any crystals once its room temp, cover the top with aluminum foil and poke a couple holes in it. Let that sit for a day or two to slowly evap, that will give you very nice crystals.

Feoom wrote:
1 Solvent (water) that mix with solvent 2 (ethanol or other solvent) 100%. But solvent 1 (water) needs to keep Freebase DMT undissolved (even at boiling point) and Solvent 2 needs to dissolve Freebase DMT at room temperature for this to work. The idea is that mixed Solvent 1 (water) + Solvent 2 kicks the recrystallization into progress.

I hope this explains a bit of what i am trying, otherwise studie the video's i have posted to make it more sense to you.


What you are describing is dual-solvent re-x, but you don't add the low solubility solvent to kick off the crystallization, that's crash precipitating, not re-x. You want to add just enough so that you see no precipitation when its near boiling, same idea as above.

Even if you found a better solvent mix than heptane, growing good crystals still takes time.


When I am recrystallizing organic compounds in the lab, I always start with ethyl acetate and heptane or hexanes. Typically things are very soluble in ethyl acetate and very insoluble in hexanes. It can be a pain to find that best ratio for each different compound. It is a godsend when one solvent alone works well. Especially when its hexanes (or heptane). Don't knock heptane so fast! try it again

And also, safety-wise, its no joke. Years ago a member on here almost burnt their house down following some bad advice... So seriously, its not all about you.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
Running Bear
#33 Posted : 1/8/2017 12:38:48 AM

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Mindlusion wrote:
[quote=Feoom]


And also, safety-wise, its no joke. Years ago a member on here almost burnt their house down following some bad advice... So seriously, its not all about you.


Dude your talking to a guy that uses laboratory glass, a magnetic stirrer with hot plate, and a separation funnel. I shouldn't have said to use a crockpot but to be completely honest with you I would be very, VERY shocked if someone burned down there house with 50cc on naphtha and a crockpot. I'm done arguing lol.
 
Feoom
#34 Posted : 1/8/2017 1:21:21 AM
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Mindlusion
#35 Posted : 1/13/2017 1:24:05 AM

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Feoom wrote:

The recrystallization proces should happen very fast (+-20/30 minutes) since if you add the minimal amount of solvents the solvents containing the Freebase DMT wants to crash out when temperature decreases. But for this technique (1 solvent, heptane in this example) to work The Freebase DMT must be undissolved in heptane at room temp but completely dissolved at near the boiling point. I don't know if that is the case with heptane. I know it dissolves at higher temps but it needs to be undissolved at room temp for the crash out of crystals to happen.



Heptane DOES do this. Sounds like you just used too much. It certainly will start to crystallize out at room temperature if you have the right concentration.

It won't all come out at once of course, but this is what you want. The best way is to put some foil over the top of the flask to slow the evaporation. This crude technique is still used in advanced organic laboratories all over the world. More complex does not equal better. In undergrad I had a fellow who worked in the lab who tried to 'improve' every procedure by adding things, mixing solvents, without first fully exploring the method he was using. He overlooked a lot of things, not fully understanding the chemistry. He never once succeeded with his 'improvements' either.

Don't get me wrong, I'm not trying to say that you shouldn't try anything new, 'stick with what works' mentality. I am saying that you should not be so quick to jump the gun.
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
benzyme
#36 Posted : 1/13/2017 5:21:30 AM

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does anyone use hexanes?

yeah, I already know... blah blah blah toxicity, blah blah blah. you're not bathing in it.
it's an effective re-x solvent, that evaporates easier than heptane. one could also freeze precip easily.
or, you could try sonocrystallization, and grow some impressive crystals, in a binary solvent system...maybe hexane and cyclohexane.

alternatively, supercritical co2 has the same polarity (of lack thereof) as hexanes.
an ideal scheme would be acidify/STB, extract with dcm, recrystallize with n-hexane. it's more effective than what is proposed in those videos. the point is to extract with a solvent that has a similar partition coefficient as the solute, and recrystallize with a solvent that has a much higher partition coeff. acetone, water, and alcohols have low partition coefficients, and thus are less effective at recrystallizing as the light aliphatics.
"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
 
Feoom
#37 Posted : 1/13/2017 7:49:00 PM
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benzyme
#38 Posted : 1/13/2017 11:12:46 PM

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honestly, I've never tried it.
as a freebase, (for crystal resolution's sake, long-term) I would be concerned of the pyrolle's hydrogen participating in h-bond interactions with an alcohol, or even acetone, as well as their propensities for absorbing ambient moisture.

generally, people even dry their nonpolar solvents, to help improve the resolution of the final product. an alcohol may leave a resinous product


"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
 
Feoom
#39 Posted : 1/13/2017 11:28:35 PM
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syberdelic
#40 Posted : 1/14/2017 2:33:08 AM

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I don't want to dissuade people from trying new things and possibly finding something better. I am pro-change in many ways.

BUT... ...

I have some experience working with a particular impatient individual on an A/B extraction. I had a tried and true method, but he couldn't leave well enough alone. It was just too slow for him and the resulting alterations to my method resulted in nothing but money down the drain and wasted effort.

My opinion is that the entire process is slow and requires patience.

Recrystalization in particular is an exercise in patience and faith. I have a fair amount of experience in forming crystals not just from chemicals in solution, but also hardening steel blades and even dark chocolate.

Naphtha, although crude is a very effective recrystalization agent for freebase DMT, providing excellent solubility at room temperature and almost complete insolubility at temperatures that any freezer can provide. And besides, if you want large crystals, you need to slow it down. You could simply dissolve the DMT, throw it in the freezer, come back in a few hours and have lots of small crystals and it's super simple.

No matter what solvent you use, if you want large pure crystals, you have to tend it meticulously. Start for an hour or two in the refrigerator. After the solution has stabilized at that temperature, put it in the freezer for 20-30 minutes and put it back in the refrigerator for another 20-30 minutes. Just keep it going back and forth until you see a few small crystals starting to precipitate out of solution.

Now you have seeds and this is where the art form begins. You don't want to "crash" it out of solution. You want the micro crystals that aren't even visible to attach themselves to the seeds. You want the entire surface of the growing seeds to stay in flux, going back and forth between soluble and insoluble. This way, the particles crashing out of solution "glue" themselves to the seed in a way that it's all one single crystal. You have three chambers to move the solution between to acheive this, room temp, refrigerator, and freezer.

I know it's counter intuitive. Someone will want to say, "can't we just find the right temperature and leave it be?" The answer is no. You need the temperature to fluctuate just slightly above and just slightly below this magic temperature so that the surface of the seed keeps melting away just a bit. When you start noticing nice uniform crystals forming, you can become a bit more lax as now your seeds have a more solid template and incoming "snow" will be much more likely to follow suit.

I have done this a few times and got nearly white crystals. As they are exposed to the air, they will inevitably turn a little yellow.
 
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