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tekkie
- Thread starter Feoom
- Start date
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...
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 said:
It would not work. When you mix sodium chloride solution and ethanol, the ethanol instantly causes the salt to drop out of solution.Diazin said:
downwardsfromzero
Boundary condition
Feoom said:
Good crystallisation takes time. It's a fact of life. Why the hurry?
Ruining Beer said:
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"
Diazin said:
Adding ethanol to saturated saline will produce nice crystals... of sodium chloride. Aim for slightly below saturation if you're trying this.
Surprise: Ethanol, or at least its inevitable metabolic product acetaldehyde, is a known carcinogen.Diazin said:
Alcohol and cancer - Wikipedia
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.downwardsfromzero said:Ruining Beer said:
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"
I'm confident that tomorrow, Running Bear will resent the lapse of better sense.
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.Feoom said:
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
).
downwardsfromzero
Boundary condition
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.pitubo said:
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.Feoom said:
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".)
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 said:
If I were to attempt to recrystallize dmt from an English ale, would I ruin the dmt or would I be ruining the beer? :lol:downwardsfromzero said:
Feoom said:
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 said:
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.
Feoom said:
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.
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.
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.
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
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
syberdelic
Rising Star
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.
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.